Selective and catalytic carbon dioxide and heteroallene activation mediated by cerium N-heterocyclic carbene complexes.
Arnold, Polly L.; Kerr, Ryan W. F.; Weetman, Catherine; Docherty, Scott R.; Rieb, Julia; Cruickshank, Faye L.; Wang, Kai; Jandl, Christian; McMullon, Max W.; Pöthig, Alexander; Kühn, Fritz E; Smith, Andrew D.; Chemical science 9 (2018) 8035–8045; doi:10.1039/c8sc03312a

data_1549913
_publ_section_title
;
 Selective and catalytic carbon dioxide and heteroallene activation
 mediated by cerium N-heterocyclic carbene complexes.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              8035
_journal_page_last               8045
_journal_paper_doi               10.1039/c8sc03312a
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C63 H87 Ce N6 O9, C7 H8, 0.5(C6 H14)'
_chemical_formula_sum            'C76 H99 Ce N6 O9'
_chemical_formula_weight         1380.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-07-15 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                62.686(2)
_cell_angle_beta                 69.389(3)
_cell_angle_gamma                77.518(3)
_cell_formula_units_Z            2
_cell_length_a                   15.9574(7)
_cell_length_b                   17.7857(4)
_cell_length_c                   17.8098(5)
_cell_measurement_reflns_used    30926
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      75.5500
_cell_measurement_theta_min      3.9250
_cell_volume                     4194.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -68.00  29.00   1.00    5.00    --  -41.42  57.00-150.00   97
  2  \w   -112.00 -15.00   1.00    5.00    --  -41.42 -57.00  60.00   97
  3  \w   -127.00 -34.00   1.00    5.00    --  -41.42 178.00 -90.00   93
  4  \w    -64.00  31.00   1.00    5.00    --  -41.42  38.00  30.00   95
  5  \w   -114.00 -19.00   1.00    5.00    --  -41.42 -38.00-120.00   95
  6  \w     57.00 128.00   1.00    5.00    --   41.42 178.00  30.00   71
  7  \w     57.00 128.00   1.00    5.00    --   41.42 178.00-150.00   71
  8  \w     87.00 178.00   1.00   20.00    --  111.00  30.00-180.00   91
  9  \w     39.00 121.00   1.00   20.00    --  111.00-125.00-150.00   82
 10  \w     37.00 142.00   1.00   20.00    --  111.00 -77.00 150.00  105
 11  \w     39.00 121.00   1.00   20.00    --  111.00-125.00  90.00   82
 12  \w     39.00 121.00   1.00   20.00    --  111.00-125.00 -30.00   82
 13  \w     40.00 135.00   1.00   20.00    --  111.00 -45.00-180.00   95
 14  \w     87.00 178.00   1.00   20.00    --  111.00  45.00-150.00   91
 15  \w     66.00 178.00   1.00   20.00    --  111.00  15.00 -60.00  112
 16  \w     87.00 178.00   1.00   20.00    --  111.00  30.00 120.00   91
 17  \w     39.00 121.00   1.00   20.00    --  111.00-125.00-120.00   82
 18  \w     88.00 178.00   1.00   20.00    --  111.00  41.00 141.34   90
 19  \w     39.00 121.00   1.00   20.00    --  111.00-125.00 150.00   82
 20  \w     39.00 121.00   1.00   20.00    --  111.00-125.00-180.00   82
 21  \w     37.00 142.00   1.00   20.00    --  111.00 -77.00 -30.00  105
 22  \w     39.00 121.00   1.00   20.00    --  111.00-125.00 -60.00   82
 23  \w     39.00 121.00   1.00   20.00    --  111.00-125.00   0.00   82
 24  \w     94.00 178.00   1.00   20.00    --  111.00 125.00-180.00   84
 25  \w     94.00 178.00   1.00   20.00    --  111.00 125.00 120.00   84
 26  \w     37.00 142.00   1.00   20.00    --  111.00 -77.00  90.00  105
 27  \w     36.00 135.00   1.00   20.00    --  111.00 -30.00-150.00   99
 28  \w     87.00 178.00   1.00   20.00    --  111.00  30.00  60.00   91
 29  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00  30.00   79
 30  \w     40.00 135.00   1.00   20.00    --  111.00 -45.00   0.00   95
 31  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00-120.00   79
 32  \w     39.00 121.00   1.00   20.00    --  111.00-125.00  30.00   82
 33  \w   -115.00 -10.00   1.00    5.00    --  -41.42 -77.00   0.00  105
 34  \w   -115.00 -10.00   1.00    5.00    --  -41.42 -77.00 -90.00  105
 35  \w   -115.00 -10.00   1.00    5.00    --  -41.42 -77.00 120.00  105
 36  \w   -115.00 -10.00   1.00    5.00    --  -41.42 -77.00  60.00  105
 37  \w   -115.00 -10.00   1.00    5.00    --  -41.42 -77.00-180.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1004620000
_diffrn_orient_matrix_UB_12      0.0174384000
_diffrn_orient_matrix_UB_13      0.0059213000
_diffrn_orient_matrix_UB_21      0.0234116000
_diffrn_orient_matrix_UB_22      0.0662705000
_diffrn_orient_matrix_UB_23      -0.0968081000
_diffrn_orient_matrix_UB_31      0.0066452000
_diffrn_orient_matrix_UB_32      -0.0696352000
_diffrn_orient_matrix_UB_33      -0.0308400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84368
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.793
_diffrn_reflns_theta_min         3.490
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.595
_exptl_absorpt_correction_T_max  0.4719
_exptl_absorpt_correction_T_min  0.3224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       block
_exptl_crystal_F_000             1454
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.143
_refine_diff_density_max         2.886
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         17387
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0966
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+33.2210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2589
_refine_ls_wR_factor_ref         0.2718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14813
_reflns_number_total             17387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03312a2.cif
_cod_data_source_block           po17034_sq
_cod_depositor_comments
;

2019-05-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1549909--1549914.cif.
;
_cod_original_formula_moiety     '2(C63 H87 Ce N6 O9), 2(C7 H8), C6 H14'
_cod_original_formula_sum        'C152 H198 Ce2 N12 O18'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     2761.45
_cod_database_code               1549913
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C60 H87 Ce N6 O3'
_chemical_oxdiff_usercomment     '@ 120 K RK'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C6S, C5S, C4S, C3S, C7S, C2S, C1S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10S, C9S, C8S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C6S \\sim C5S \\sim C4S \\sim C3S \\sim C7S \\sim C2S \\sim C1S: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C8S \\sim C9S \\sim C10S: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 C10S, C9S, C8S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C60(H60), C50(H50), C70(H70)
5.b Secondary CH2 refined with riding coordinates:
 C8S(H8SA,H8SB), C9S(H9SA,H9SB)
5.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C27(H27), C22(H22), C32(H32), C33(H33), C19(H19), C23(H23),
 C39(H39), C37(H37), C17(H17), C12(H12), C13(H13), C4S(H4S), C3S(H3S), C7S(H7S),
  C6S(H6S), C5S(H5S)
5.d Fitted pentagon refined as free rotating group:
 N6(C31,N5,C32,C33)
5.e Fitted hexagon refined as free rotating group:
 C4S(C3S,C2S,C7S,C6S,C5S)
5.f Idealised Me refined as rotating group:
 C263(H26A,H26B,H26C), C262(H26D,H26E,H26F), C62(H62A,H62B,H62C), C282(H28A,
 H28B,H28C), C283(H28D,H28E,H28F), C281(H28G,H28H,H28I), C161(H16A,H16B,H16C),
 C361(H36A,H36B,H36C), C363(H36D,H36E,H36F), C362(H36G,H36H,H36I), C261(H26G,
 H26H,H26I), C162(H16D,H16E,H16F), C61(H61A,H61B,H61C), C163(H16G,H16H,H16I),
 C381(H38A,H38B,H38C), C183(H18A,H18B,H18C), C71(H71A,H71B,H71C), C51(H51A,H51B,
 H51C), C181(H18D,H18E,H18F), C52(H52A,H52B,H52C), C182(H18G,H18H,H18I),
 C383(H38D,H38E,H38F), C72(H72A,H72B,H72C), C382(H38G,H38H,H38I), C1S(H1SA,H1SB,
 H1SC), C10S(H10A,H10B,H10C)
;
_shelx_res_checksum              54103
_shelxl_res_file
;
TITL po17034_a.res in P-1
    po17034_sq.res
    created by SHELXL-2016/6 at 14:03:43 on 11-Aug-2017
REM Old TITL
REM SHELXT solution in P-1
REM R1 0.209, Rweak 0.043, Alpha 0.069, Orientation as input
REM Formula found by SHELXT: C68 Ce N8 O10
CELL 1.54184 15.9574 17.7857 17.8098 62.686 69.389 77.518
ZERR 1 0.0007 0.0004 0.0005 0.002 0.003 0.003
LATT 1
SFAC C H Ce N O
UNIT 152 198 2 12 18
DELU C6S C5S C4S C3S C7S C2S C1S
DELU C10S C9S C8S
SIMU C6S C5S C4S C3S C7S C2S C1S
SIMU C8S C9S C10S
RIGU C10S C9S C8S

L.S. 100 0 97
PLAN  15
BOND $H
list 4
ABIN
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\po17034.hkl">
REM </olex2.extras>

WGHT    0.140000   33.221001
FVAR       0.33846
CE1   3    0.637526    0.321198    0.282438    11.00000    0.06102    0.02722 =
         0.03710   -0.01449   -0.00753   -0.00622
O21   5    0.721462    0.430801    0.174176    11.00000    0.06912    0.03536 =
         0.04195   -0.01659   -0.00806   -0.00835
O13   5    0.509855    0.238145    0.325014    11.00000    0.06904    0.04382 =
         0.04450   -0.02163   -0.00090   -0.01424
O31   5    0.722588    0.280413    0.374233    11.00000    0.08023    0.03528 =
         0.04905   -0.01598   -0.01172   -0.00439
O11   5    0.696238    0.226315    0.220421    11.00000    0.06173    0.04171 =
         0.05546   -0.02297   -0.01088   -0.00475
O33   5    0.534589    0.340562    0.413792    11.00000    0.08228    0.04291 =
         0.05146   -0.02712   -0.00502   -0.00590
O23   5    0.527212    0.430656    0.215989    11.00000    0.07596    0.03857 =
         0.06939   -0.02150   -0.02762   -0.00470
N4    4    0.508955    0.555120    0.311390    11.00000    0.06185    0.03141 =
         0.03699   -0.01839   -0.00473   -0.00169
O12   5    0.507224    0.119551    0.311641    11.00000    0.12554    0.03423 =
         0.05051   -0.01546   -0.00719   -0.02469
N3    4    0.636007    0.571588    0.208009    11.00000    0.06518    0.04276 =
         0.04266   -0.02521   -0.00351   -0.00424
O32   5    0.524778    0.317631    0.549073    11.00000    0.15479    0.05928 =
         0.06314   -0.04385   -0.03491    0.01960
N1    4    0.471278    0.309535    0.146384    11.00000    0.08922    0.04728 =
         0.08278   -0.01776   -0.05210   -0.00422
C24   1    0.702150    0.579252    0.125587    11.00000    0.05381    0.03795 =
         0.04618   -0.02422   -0.00012   -0.00399
C25   1    0.741413    0.506568    0.110373    11.00000    0.05352    0.03259 =
         0.04008   -0.01812   -0.00863   -0.00368
C29   1    0.723093    0.662098    0.064419    11.00000    0.05700    0.03664 =
         0.05523   -0.02715   -0.00761   -0.00054
AFIX  43
H29   2    0.694562    0.707614    0.078058    11.00000   -1.20000
AFIX   0
O22   5    0.476814    0.558676    0.142247    11.00000    0.15659    0.05471 =
         0.07224   -0.01706   -0.06735    0.00389
C27   1    0.823243    0.604692   -0.034460    11.00000    0.05307    0.03415 =
         0.04676   -0.02228   -0.00233   -0.00857
AFIX  43
H27   2    0.864240    0.613236   -0.089424    11.00000   -1.20000
AFIX   0
C21   1    0.553545    0.543795    0.237166    11.00000    0.06046    0.03475 =
         0.04040   -0.01565   -0.00508   -0.00349
C34   1    0.708427    0.188709    0.527303    11.00000    0.08862    0.03739 =
         0.04546   -0.01640   -0.02025    0.00683
C20   1    0.516240    0.508889    0.193374    11.00000    0.06211    0.04504 =
         0.04227   -0.01486   -0.00992   -0.00399
N2    4    0.594041    0.234562    0.120463    11.00000    0.07766    0.06166 =
         0.04240   -0.02057   -0.01781   -0.00880
C26   1    0.802113    0.522333    0.024787    11.00000    0.05277    0.03317 =
         0.03808   -0.01662   -0.00745   -0.00384
C14   1    0.667485    0.172627    0.134066    11.00000    0.06260    0.05428 =
         0.05185   -0.03312   -0.01007    0.00010
C28   1    0.786610    0.676190   -0.016732    11.00000    0.05891    0.02833 =
         0.04552   -0.01660   -0.00831   -0.00519
C263  1    0.905943    0.477525   -0.097175    11.00000    0.07557    0.04521 =
         0.05362   -0.02927    0.00423   -0.00861
AFIX 137
H26A  2    0.869640    0.513198   -0.135286    11.00000   -1.50000
H26B  2    0.931386    0.429337   -0.110356    11.00000   -1.50000
H26C  2    0.953253    0.508971   -0.106322    11.00000   -1.50000
AFIX   0
C30   1    0.536946    0.296345    0.491336    11.00000    0.06936    0.05092 =
         0.05630   -0.03569    0.00186   -0.01454
C15   1    0.716164    0.169813    0.186521    11.00000    0.06270    0.04764 =
         0.05452   -0.02921   -0.00331   -0.00926
C22   1    0.641784    0.601356    0.264796    11.00000    0.07295    0.05940 =
         0.06069   -0.03905   -0.00332   -0.01220
AFIX  43
H22   2    0.691762    0.624014    0.259984    11.00000   -1.20000
AFIX   0
C10   1    0.513493    0.195840    0.282914    11.00000    0.06141    0.04006 =
         0.05681   -0.01925   -0.00524   -0.01152
AFIX  56
N6    4    0.490810    0.147878    0.535684    11.00000    0.12911    0.05720 =
         0.05307   -0.03063    0.01140   -0.04550
C31   1    0.553095    0.204847    0.516892    11.00000    0.08646    0.04582 =
         0.04351   -0.01859    0.00758   -0.02312
N5    4    0.634495    0.157162    0.529982    11.00000    0.12036    0.02558 =
         0.04493   -0.01178   -0.01100   -0.01124
C32   1    0.622518    0.070723    0.556864    11.00000    0.11657    0.03385 =
         0.17906   -0.06511   -0.06125    0.01381
AFIX  43
H32   2    0.665319    0.025762    0.569877    11.00000   -1.20000
AFIX  55
C33   1    0.533717    0.064985    0.560388    11.00000    0.20209    0.03499 =
         0.04357   -0.00610   -0.00062   -0.04050
AFIX  43
H33   2    0.508147    0.015607    0.576114    11.00000   -1.20000
AFIX   0
C19   1    0.685064    0.116849    0.092972    11.00000    0.08374    0.09014 =
         0.06016   -0.05611   -0.00658   -0.01247
AFIX  43
H19   2    0.650214    0.122194    0.058290    11.00000   -1.20000
AFIX   0
C262  1    0.775967    0.394476    0.012613    11.00000    0.07687    0.04024 =
         0.04503   -0.01995   -0.00591   -0.01297
AFIX 137
H26D  2    0.737409    0.375754    0.072256    11.00000   -1.50000
H26E  2    0.804403    0.346101    0.000736    11.00000   -1.50000
H26F  2    0.741118    0.428389   -0.027452    11.00000   -1.50000
AFIX   0
C280  1    0.815948    0.765447   -0.080878    11.00000    0.05892    0.03200 =
         0.05550   -0.01970   -0.00627   -0.00527
C23   1    0.562485    0.592136    0.328894    11.00000    0.07859    0.04063 =
         0.04786   -0.02407   -0.00523   -0.00380
AFIX  43
H23   2    0.547357    0.607772    0.375454    11.00000   -1.20000
AFIX   0
C39   1    0.736588    0.155587    0.598970    11.00000    0.11759    0.04557 =
         0.04893   -0.01356   -0.02696    0.01302
AFIX  43
H39   2    0.707231    0.111213    0.649613    11.00000   -1.20000
AFIX   0
C260  1    0.847078    0.446948    0.000435    11.00000    0.06053    0.03630 =
         0.04160   -0.01856   -0.00519   -0.00588
C16   1    0.785090    0.103855    0.201542    11.00000    0.05894    0.05016 =
         0.07530   -0.03698   -0.00649   -0.00588
C160  1    0.840095    0.093211    0.260715    11.00000    0.06211    0.04665 =
         0.07743   -0.03058   -0.01690   -0.00345
C11   1    0.526165    0.246952    0.184389    11.00000    0.06920    0.04485 =
         0.05019   -0.01837   -0.01909   -0.00482
C62   1    0.398294    0.501950    0.457923    11.00000    0.09122    0.05278 =
         0.04435   -0.01752    0.00736   -0.00901
AFIX 137
H62A  2    0.433187    0.449032    0.476168    11.00000   -1.50000
H62B  2    0.335891    0.492724    0.488424    11.00000   -1.50000
H62C  2    0.416632    0.540950    0.471706    11.00000   -1.50000
AFIX   0
C282  1    0.868377    0.793884   -0.042016    11.00000    0.08921    0.05309 =
         0.06917   -0.03917   -0.01328   -0.01211
AFIX 137
H28A  2    0.833590    0.786801    0.016821    11.00000   -1.50000
H28B  2    0.880352    0.852510   -0.078144    11.00000   -1.50000
H28C  2    0.924046    0.760163   -0.040369    11.00000   -1.50000
AFIX   0
C35   1    0.751403    0.256173    0.443472    11.00000    0.06875    0.03871 =
         0.04544   -0.01918   -0.01667    0.00956
C37   1    0.850001    0.254972    0.519851    11.00000    0.08047    0.08559 =
         0.05884   -0.03943   -0.02797    0.02048
AFIX  43
H37   2    0.898325    0.277135    0.518807    11.00000   -1.20000
AFIX   0
C18   1    0.754157    0.054322    0.104416    11.00000    0.07487    0.09961 =
         0.09597   -0.08043   -0.00680   -0.00168
C60   1    0.412649    0.538166    0.360069    11.00000    0.06254    0.06337 =
         0.05002   -0.02194   -0.00092   -0.00892
AFIX  13
H60   2    0.395517    0.497385    0.346163    11.00000   -1.20000
AFIX   0
C283  1    0.733215    0.827890   -0.092740    11.00000    0.08126    0.03094 =
         0.08111   -0.00984   -0.01488    0.00346
AFIX 137
H28D  2    0.693226    0.805924   -0.106325    11.00000   -1.50000
H28E  2    0.751917    0.881657   -0.140166    11.00000   -1.50000
H28F  2    0.702891    0.835042   -0.039127    11.00000   -1.50000
AFIX   0
C360  1    0.871353    0.366011    0.360954    11.00000    0.06958    0.06847 =
         0.05774   -0.02585   -0.01527   -0.00975
C50   1    0.386676    0.342948    0.195861    11.00000    0.07136    0.06262 =
         0.15749   -0.05929   -0.05626    0.01625
AFIX  13
H50   2    0.399278    0.350641    0.241841    11.00000   -1.20000
AFIX   0
C281  1    0.875043    0.772160   -0.173055    11.00000    0.07014    0.04237 =
         0.05965   -0.01538   -0.00155   -0.01718
AFIX 137
H28G  2    0.925940    0.731981   -0.167174    11.00000   -1.50000
H28H  2    0.895272    0.828444   -0.208749    11.00000   -1.50000
H28I  2    0.840712    0.760236   -0.200632    11.00000   -1.50000
AFIX   0
C161  1    0.778359    0.078384    0.354422    11.00000    0.08101    0.03904 =
         0.08072   -0.01555   -0.03002   -0.00501
AFIX 137
H16A  2    0.739680    0.128378    0.352344    11.00000   -1.50000
H16B  2    0.814236    0.066137    0.392594    11.00000   -1.50000
H16C  2    0.742712    0.031402    0.376688    11.00000   -1.50000
AFIX   0
C38   1    0.809321    0.186761    0.598632    11.00000    0.10888    0.05856 =
         0.04208   -0.01510   -0.03044    0.02873
C17   1    0.801927    0.048575    0.161249    11.00000    0.06618    0.08372 =
         0.10435   -0.07312   -0.00354   -0.00362
AFIX  43
H17   2    0.846957    0.005491    0.172155    11.00000   -1.20000
AFIX   0
C12   1    0.580752    0.291004    0.040313    11.00000    0.12343    0.09594 =
         0.04341   -0.01161   -0.03280   -0.02960
AFIX  43
H12   2    0.618274    0.295941   -0.015006    11.00000   -1.20000
AFIX   0
C361  1    0.916683    0.337765    0.285881    11.00000    0.07911    0.08285 =
         0.05684   -0.03393   -0.01215   -0.01325
AFIX 137
H36A  2    0.871972    0.322114    0.271965    11.00000   -1.50000
H36B  2    0.958208    0.289928    0.303937    11.00000   -1.50000
H36C  2    0.948306    0.383532    0.234645    11.00000   -1.50000
AFIX   0
C363  1    0.802068    0.440266    0.336477    11.00000    0.08747    0.05106 =
         0.06731   -0.01293   -0.02321   -0.01442
AFIX 137
H36D  2    0.829135    0.484333    0.280454    11.00000   -1.50000
H36E  2    0.781184    0.461822    0.380904    11.00000   -1.50000
H36F  2    0.752371    0.421281    0.332701    11.00000   -1.50000
AFIX   0
C13   1    0.505645    0.336600    0.055947    11.00000    0.13740    0.06422 =
         0.08015   -0.00406   -0.07387   -0.00875
AFIX  43
H13   2    0.480194    0.379376    0.013763    11.00000   -1.20000
AFIX   0
C36   1    0.822940    0.290741    0.444695    11.00000    0.07311    0.05120 =
         0.04138   -0.01977   -0.01646    0.00612
C362  1    0.944968    0.395792    0.375651    11.00000    0.09748    0.10815 =
         0.07093   -0.03852   -0.02447   -0.02126
AFIX 137
H36G  2    0.988522    0.349557    0.392328    11.00000   -1.50000
H36H  2    0.918906    0.415059    0.421781    11.00000   -1.50000
H36I  2    0.973658    0.441442    0.322062    11.00000   -1.50000
AFIX   0
C261  1    0.907064    0.391552    0.059011    11.00000    0.06910    0.04486 =
         0.06207   -0.02669   -0.01533    0.00765
AFIX 137
H26G  2    0.957536    0.422090    0.044234    11.00000   -1.50000
H26H  2    0.927895    0.340745    0.049810    11.00000   -1.50000
H26I  2    0.873509    0.376962    0.119849    11.00000   -1.50000
AFIX   0
C162  1    0.891076    0.171763    0.223819    11.00000    0.06768    0.07023 =
         0.09518   -0.03946   -0.01200   -0.01794
AFIX 137
H16D  2    0.934055    0.178392    0.167933    11.00000   -1.50000
H16E  2    0.921665    0.165607    0.264279    11.00000   -1.50000
H16F  2    0.849653    0.220822    0.215981    11.00000   -1.50000
AFIX   0
C61   1    0.356505    0.621670    0.328588    11.00000    0.07353    0.09281 =
         0.06986   -0.02431   -0.01048    0.01574
AFIX 137
H61A  2    0.376988    0.663535    0.336808    11.00000   -1.50000
H61B  2    0.294605    0.613107    0.362095    11.00000   -1.50000
H61C  2    0.362665    0.640808    0.267092    11.00000   -1.50000
AFIX   0
C163  1    0.910522    0.017369    0.270137    11.00000    0.09356    0.09461 =
         0.14199   -0.07454   -0.05281    0.02554
AFIX 137
H16G  2    0.881585   -0.033149    0.289586    11.00000   -1.50000
H16H  2    0.938913    0.010160    0.312628    11.00000   -1.50000
H16I  2    0.954889    0.027905    0.214059    11.00000   -1.50000
AFIX   0
C381  1    0.932900    0.167713    0.659816    11.00000    0.20416    0.08470 =
         0.06653   -0.00801   -0.08246    0.02088
AFIX 137
H38A  2    0.972455    0.141677    0.622230    11.00000   -1.50000
H38B  2    0.949755    0.146512    0.713069    11.00000   -1.50000
H38C  2    0.937037    0.228066    0.629717    11.00000   -1.50000
AFIX   0
C183  1    0.716615    0.005239    0.008394    11.00000    0.10764    0.18576 =
         0.15478   -0.14846   -0.01823    0.00039
AFIX 137
H18A  2    0.655578    0.009450    0.042935    11.00000   -1.50000
H18B  2    0.724890   -0.040990   -0.007848    11.00000   -1.50000
H18C  2    0.729836    0.057105   -0.043990    11.00000   -1.50000
AFIX   0
C380  1    0.840060    0.147601    0.681945    11.00000    0.11243    0.08324 =
         0.07356   -0.03158   -0.04977    0.03199
C71   1    0.367404    0.114721    0.511081    11.00000    0.18378    0.16953 =
         0.09967   -0.07598    0.04310   -0.13468
AFIX 137
H71A  2    0.407130    0.114733    0.456171    11.00000   -1.50000
H71B  2    0.308149    0.134845    0.505260    11.00000   -1.50000
H71C  2    0.365942    0.058100    0.556773    11.00000   -1.50000
AFIX   0
C51   1    0.353011    0.426853    0.135680    11.00000    0.15856    0.07126 =
         0.33209   -0.07262   -0.17101    0.04074
AFIX 137
H51A  2    0.398102    0.466954    0.108808    11.00000   -1.50000
H51B  2    0.299491    0.447137    0.169210    11.00000   -1.50000
H51C  2    0.339920    0.420104    0.090552    11.00000   -1.50000
AFIX   0
C180  1    0.779502   -0.010427    0.062608    11.00000    0.09907    0.11661 =
         0.10049   -0.08688   -0.00292   -0.00702
C181  1    0.769207   -0.098425    0.133694    11.00000    0.14666    0.09966 =
         0.12718   -0.08994    0.01176   -0.02814
AFIX 137
H18D  2    0.803195   -0.107736    0.172582    11.00000   -1.50000
H18E  2    0.790783   -0.138351    0.107672    11.00000   -1.50000
H18F  2    0.707018   -0.105814    0.166573    11.00000   -1.50000
AFIX   0
C70   1    0.400653    0.172506    0.534898    11.00000    0.08914    0.15190 =
         0.11829   -0.10084    0.04601   -0.06992
AFIX  13
H70   2    0.396585    0.231234    0.491265    11.00000   -1.20000
AFIX   0
C52   1    0.317386    0.276016    0.240411    11.00000    0.06525    0.11961 =
         0.25541   -0.11261   -0.03247   -0.00653
AFIX 137
H52A  2    0.313248    0.259610    0.197514    11.00000   -1.50000
H52B  2    0.259921    0.299293    0.264815    11.00000   -1.50000
H52C  2    0.335630    0.227263    0.286780    11.00000   -1.50000
AFIX   0
C182  1    0.874386    0.003649    0.002667    11.00000    0.09386    0.16112 =
         0.17048   -0.13989    0.01816   -0.01755
AFIX 137
H18G  2    0.878049    0.061498   -0.040511    11.00000   -1.50000
H18H  2    0.891268   -0.033447   -0.026682    11.00000   -1.50000
H18I  2    0.914226   -0.008146    0.037046    11.00000   -1.50000
AFIX   0
C383  1    0.840907    0.054961    0.726432    11.00000    0.17375    0.09867 =
         0.07853    0.01964   -0.08303   -0.00703
AFIX 137
H38D  2    0.781857    0.037550    0.742356    11.00000   -1.50000
H38E  2    0.859120    0.035268    0.778722    11.00000   -1.50000
H38F  2    0.882298    0.031308    0.687395    11.00000   -1.50000
AFIX   0
C72   1    0.346441    0.166535    0.625544    11.00000    0.13150    0.48099 =
         0.18699   -0.26485    0.06656   -0.11207
AFIX 137
H72A  2    0.354550    0.110134    0.668820    11.00000   -1.50000
H72B  2    0.284113    0.179351    0.628285    11.00000   -1.50000
H72C  2    0.366080    0.206310    0.637349    11.00000   -1.50000
AFIX   0
C382  1    0.781622    0.190105    0.743073    11.00000    0.27903    0.27688 =
         0.08150   -0.11035   -0.12117    0.17982
AFIX 137
H38G  2    0.799913    0.246385    0.720226    11.00000   -1.50000
H38H  2    0.788606    0.157524    0.801162    11.00000   -1.50000
H38I  2    0.719846    0.192954    0.746012    11.00000   -1.50000
AFIX  66

C4S   1    0.517618    0.822095    0.225567    11.00000    0.26111    0.16432 =
         0.13452   -0.09014    0.03962   -0.05646
AFIX  43
H4S   2    0.541769    0.775781    0.266322    11.00000   -1.20000
AFIX  65
C3S   1    0.498462    0.899360    0.231949    11.00000    0.17672    0.15014 =
         0.08144   -0.06246    0.02822   -0.03578
AFIX  43
H3S   2    0.509797    0.904740    0.276973    11.00000   -1.20000
AFIX  65
C2S   1    0.462366    0.968582    0.171036    11.00000    0.10697    0.19378 =
         0.12058   -0.07854    0.00755   -0.05196
C7S   1    0.445424    0.960541    0.103742    11.00000    0.15518    0.17560 =
         0.13178   -0.07319   -0.01297   -0.04457
AFIX  43
H7S   2    0.421273    1.006855    0.062987    11.00000   -1.20000
AFIX  65
C6S   1    0.464579    0.883277    0.097359    11.00000    0.21445    0.16520 =
         0.19295   -0.08277    0.00056   -0.07357
AFIX  43
H6S   2    0.453244    0.877897    0.052335    11.00000   -1.20000
AFIX  65
C5S   1    0.500676    0.814054    0.158271    11.00000    0.19411    0.16084 =
         0.21412   -0.09743   -0.01696   -0.06422
AFIX  43
H5S   2    0.513492    0.762359    0.154001    11.00000   -1.20000
AFIX   0
C1S   1    0.450254    1.053654    0.185480    11.00000    0.14274    0.15702 =
         0.11904   -0.05384   -0.02898   -0.01843
AFIX 137
H1SA  2    0.490118    1.049116    0.217286    11.00000   -1.50000
H1SB  2    0.389413    1.061106    0.218654    11.00000   -1.50000
H1SC  2    0.464003    1.101501    0.129120    11.00000   -1.50000
AFIX   0

C8S   1    0.949059    0.982220   -0.485395    11.00000    0.23133    0.16912 =
         0.12736   -0.06549   -0.12345    0.02499
AFIX  23
H8SA  2    0.903488    1.007481   -0.449192    11.00000   -1.20000
H8SB  2    0.931642    0.994333   -0.537009    11.00000   -1.20000
AFIX   0
C9S   1    0.962644    0.893610   -0.436649    11.00000    0.20802    0.16010 =
         0.12837   -0.08948   -0.08585    0.04904
AFIX  23
H9SA  2    0.974991    0.881302   -0.382419    11.00000   -1.20000
H9SB  2    1.011764    0.869199   -0.471246    11.00000   -1.20000
AFIX   0
C10S  1    0.867284    0.858047   -0.416067    11.00000    0.26610    0.26688 =
         0.16913   -0.08336   -0.04642   -0.06326
AFIX 137
H10A  2    0.818856    0.891253   -0.392663    11.00000   -1.50000
H10B  2    0.865336    0.799868   -0.373730    11.00000   -1.50000
H10C  2    0.861536    0.862090   -0.469695    11.00000   -1.50000
AFIX   0
HKLF 4

REM  po17034_a.res in P-1
REM R1 =  0.0966 for   14813 Fo > 4sig(Fo)  and  0.1098 for all   17387 data
REM    807 parameters refined using     81 restraints

END  
     
WGHT      0.1054     28.0233 

REM Highest difference peak  2.886,  deepest hole -1.600,  1-sigma level  0.123
Q1    1   0.6375  0.5368  0.0686  11.00000  0.05    2.89
Q2    1   0.6414  0.1011  0.5048  11.00000  0.05    2.26
Q3    1   0.4874  0.7766  0.0971  11.00000  0.05    2.05
Q4    1   0.7027  0.3127  0.2695  11.00000  0.05    1.95
Q5    1   0.5674  0.3256  0.3043  11.00000  0.05    1.45
Q6    1   0.6231  0.3230  0.2374  11.00000  0.05    1.35
Q7    1   0.6821  0.2970  0.3370  11.00000  0.05    1.30
Q8    1   0.5992  0.3414  0.2197  11.00000  0.05    1.16
Q9    1   0.4540  1.0121  0.1415  11.00000  0.05    1.08
Q10   1   0.3618  1.1350  0.2619  11.00000  0.05    1.05
Q11   1   0.9028  0.9314 -0.1242  11.00000  0.05    0.91
Q12   1   0.4466  0.8443  0.2021  11.00000  0.05    0.91
Q13   1   0.3637  0.2355  0.1590  11.00000  0.05    0.87
Q14   1   0.5833  0.0814  0.5678  11.00000  0.05    0.83
Q15   1   0.4841  0.9753  0.2181  11.00000  0.05    0.83

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0966 for 14813 Fo > 4sig(Fo) and 0.1098 for all 84368 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 2.89, deepest hole -1.60
  REM Mean Shift 0, Max Shift -0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.1098
  REM R1_gt = 0.0966
  REM wR_ref = 0.2718
  REM GOOF = 0.950
  REM Shift_max = -0.001
  REM Shift_mean = 0
  REM Reflections_all = 84368
  REM Reflections_gt = 14813
  REM Parameters = n/a
  REM Hole = -1.60
  REM Peak = 2.89
  REM Flack = n/a
;
_shelx_fab_checksum              15532
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.758