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_1549914
_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         'C78 H99 Ce N6 O3, C6 H6'
_chemical_formula_sum            'C84 H105 Ce N6 O3'
_chemical_formula_weight         1386.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-15 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6458(2)
_cell_length_b                   24.6116(4)
_cell_length_c                   24.4523(4)
_cell_measurement_reflns_used    13685
_cell_measurement_temperature    120.01(13)
_cell_measurement_theta_max      29.1220
_cell_measurement_theta_min      3.3840
_cell_volume                     7593.6(2)
_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      120.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.888
_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     -3.00  23.00   1.00   30.00    --  -16.47  77.00  90.00   26
  2  \w    -45.00  -7.00   1.00   30.00    --  -16.47  77.00  90.00   38
  3  \w     46.00  86.00   1.00   30.00    --   18.03  57.00  30.00   40
  4  \w     -5.00  80.00   1.00   30.00    --   18.03  37.00 -30.00   85
  5  \w     34.00  70.00   1.00   30.00    --   18.03 179.00  30.00   36
  6  \w     -1.00  66.00   1.00   30.00    --   18.03  77.00   0.00   67
  7  \w    -10.00  86.00   1.00   30.00    --   18.03  77.00 150.00   96
  8  \w     43.00  89.00   1.00   30.00    --   18.03  37.00-120.00   46
  9  \w     34.00  64.00   1.00   30.00    --   18.03 179.00-180.00   30
 10  \w     31.00  59.00   1.00   30.00    --   18.03 -99.00 -90.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0035006000
_diffrn_orient_matrix_UB_12      -0.0287481000
_diffrn_orient_matrix_UB_13      -0.0005481000
_diffrn_orient_matrix_UB_21      0.0009091000
_diffrn_orient_matrix_UB_22      -0.0006340000
_diffrn_orient_matrix_UB_23      0.0290316000
_diffrn_orient_matrix_UB_31      -0.0561058000
_diffrn_orient_matrix_UB_32      -0.0018002000
_diffrn_orient_matrix_UB_33      -0.0014990000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            80664
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.338
_diffrn_reflns_theta_min         2.914
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       needle
_exptl_crystal_F_000             2932
_exptl_crystal_size_max          0.549
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         18512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13869
_reflns_number_total             18512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03312a2.cif
_cod_data_source_block           p17079
_cod_depositor_comments
'Adding full bibliography for 1549909--1549914.cif.'
_cod_database_code               1549914
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C50 H100 N6 O3 Ce1'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C383) = Uanis(C382)
3. Others
 Sof(C386)=Sof(H38J)=Sof(H38K)=Sof(H38L)=Sof(C382)=Sof(H38M)=Sof(H38N)=
 Sof(H38O)=Sof(C384)=Sof(H38P)=Sof(H38Q)=Sof(H38R)=1-FVAR(1)
 Sof(C381)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C383)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C385)=Sof(H38G)=Sof(H38H)=Sof(H38I)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C22(H22), C29(H29), C19(H19), C37(H37), C54(H54), C32(H32),
 C17(H17), C27(H27), C74(H74), C39(H39), C72(H72), C64(H64), C33(H33), C62(H62),
  C52(H52), C1S(H1S), C3S(H3S), C2S(H2S), C4S(H4S), C12(H12), C13(H13),
 C6S(H6S), C5S(H5S)
4.b Idealised Me refined as rotating group:
 C750(H75A,H75B,H75C), C362(H36A,H36B,H36C), C361(H36D,H36E,H36F), C263(H26A,
 H26B,H26C), C262(H26D,H26E,H26F), C161(H16A,H16B,H16C), C162(H16D,H16E,H16F),
 C650(H65A,H65B,H65C), C610(H61A,H61B,H61C), C163(H16G,H16H,H16I), C261(H26G,
 H26H,H26I), C363(H36G,H36H,H36I), C710(H71A,H71B,H71C), C510(H51A,H51B,H51C),
 C550(H55A,H55B,H55C), C283(H28A,H28B,H28C), C183(H18A,H18B,H18C), C530(H53A,
 H53B,H53C), C730(H73A,H73B,H73C), C630(H63A,H63B,H63C), C281(H28D,H28E,H28F),
 C181(H18D,H18E,H18F), C381(H38A,H38B,H38C), C383(H38D,H38E,H38F), C182(H18G,
 H18H,H18I), C282(H28G,H28H,H28I), C385(H38G,H38H,H38I), C386(H38J,H38K,H38L),
 C382(H38M,H38N,H38O), C384(H38P,H38Q,H38R)
;
_shelx_res_checksum              540
_shelxl_res_file
;
TITL p17079_a.res in P2(1)/c
    p17079.res
    created by SHELXL-2016/6 at 11:12:57 on 29-Jun-2018
REM Old TITL P17079 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.099, Rweak 0.009, Alpha 0.024, Orientation as input
REM Formula found by SHELXT: C81 N9 O3 Ce
CELL 0.71073 12.6458 24.6116 24.4523 90 93.8 90
ZERR 4 0.0002 0.0004 0.0004 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Ce N O
UNIT 336 420 4 24 12
EADP C383 C382

L.S. 10
PLAN  20
BOND $H
list 4
fmap 2 53
acta
OMIT 5 5 1
OMIT 6 3 0
OMIT 2 7 5
REM <olex2.extras>
REM <HklSrc "%.\\P17079.hkl">
REM </olex2.extras>

WGHT    0.100000
FVAR       0.25833   0.74262
CE01  3    0.765427    0.792671    0.440623    11.00000    0.01807    0.01438 =
         0.01289   -0.00105    0.00085   -0.00031
O21   5    0.823580    0.844522    0.372252    11.00000    0.02019    0.02086 =
         0.01684    0.00276    0.00159    0.00607
O11   5    0.894819    0.819428    0.502447    11.00000    0.02633    0.02327 =
         0.01642   -0.00313    0.00048   -0.00326
O31   5    0.847816    0.716791    0.412732    11.00000    0.02079    0.01250 =
         0.02592   -0.00372    0.00062    0.00059
N3    4    0.674922    0.928550    0.387560    11.00000    0.02077    0.01671 =
         0.01674    0.00086    0.00299    0.00205
N5    4    0.658655    0.666979    0.368408    11.00000    0.02208    0.02074 =
         0.02026   -0.00445   -0.00100   -0.00316
N4    4    0.621962    0.927555    0.468734    11.00000    0.02170    0.01536 =
         0.01710    0.00041    0.00270    0.00316
N1    4    0.782172    0.788780    0.593926    11.00000    0.04170    0.02585 =
         0.01583   -0.00014    0.00208   -0.00975
C21   1    0.663198    0.894032    0.430712    11.00000    0.01664    0.01941 =
         0.01604    0.00161    0.00301    0.00045
N6    4    0.538217    0.726680    0.349649    11.00000    0.02143    0.02452 =
         0.02337   -0.00616    0.00018   -0.00464
C11   1    0.726354    0.766796    0.549192    11.00000    0.02788    0.01934 =
         0.01565   -0.00209    0.00334   -0.00302
C25   1    0.797393    0.877918    0.331067    11.00000    0.01834    0.01710 =
         0.01666    0.00123   -0.00063   -0.00361
N2    4    0.674143    0.724793    0.571832    11.00000    0.05327    0.02903 =
         0.01697   -0.00061    0.00868   -0.01723
C31   1    0.630472    0.718929    0.381658    11.00000    0.02400    0.02096 =
         0.01635    0.00004    0.00194   -0.00072
C24   1    0.717102    0.916815    0.335356    11.00000    0.01855    0.02003 =
         0.01549   -0.00129    0.00249   -0.00038
C15   1    0.918316    0.843397    0.550339    11.00000    0.02429    0.01563 =
         0.01761   -0.00229   -0.00547    0.00215
C26   1    0.846128    0.874898    0.280366    11.00000    0.01892    0.01784 =
         0.02060    0.00176    0.00465    0.00086
C36   1    0.940763    0.631766    0.411591    11.00000    0.02755    0.01831 =
         0.01419   -0.00158   -0.00096    0.00246
C35   1    0.847039    0.664114    0.403873    11.00000    0.02386    0.02061 =
         0.01466   -0.00066    0.00054    0.00284
C60   1    0.594602    0.912547    0.523041    11.00000    0.02490    0.01580 =
         0.01948    0.00082    0.00727    0.00475
C14   1    0.859408    0.832179    0.595748    11.00000    0.03169    0.01704 =
         0.01903    0.00102   -0.00326   -0.00165
C23   1    0.608901    0.980108    0.450113    11.00000    0.02664    0.01860 =
         0.02267    0.00000    0.00421    0.00609
AFIX  43
H23   2    0.582287    1.009262    0.469122    11.00000   -1.20000
AFIX   0
C22   1    0.642163    0.980937    0.399120    11.00000    0.03169    0.01791 =
         0.02119    0.00270    0.00188    0.00587
AFIX  43
H22   2    0.643097    1.010874    0.375949    11.00000   -1.20000
AFIX   0
C16   1    1.003323    0.880760    0.558207    11.00000    0.02354    0.01863 =
         0.02396   -0.00203   -0.00495    0.00282
C29   1    0.677842    0.946983    0.290191    11.00000    0.02151    0.01875 =
         0.02190    0.00037    0.00130    0.00378
AFIX  43
H29   2    0.622098    0.971001    0.294171    11.00000   -1.20000
AFIX   0
C70   1    0.481448    0.776654    0.342581    11.00000    0.01574    0.02364 =
         0.02525   -0.00247   -0.00297   -0.00162
C19   1    0.876708    0.859922    0.645105    11.00000    0.03575    0.02649 =
         0.01625   -0.00083   -0.00081    0.00049
AFIX  43
H19   2    0.833603    0.852688    0.673606    11.00000   -1.20000
AFIX   0
C75   1    0.514179    0.813901    0.304116    11.00000    0.01961    0.02876 =
         0.02290   -0.00303   -0.00170   -0.00654
C34   1    0.752811    0.636945    0.386428    11.00000    0.02563    0.01964 =
         0.01736   -0.00473    0.00317    0.00044
C750  1    0.605671    0.801548    0.270262    11.00000    0.03276    0.03578 =
         0.02804   -0.00201    0.01119   -0.00359
AFIX 137
H75A  2    0.665849    0.790982    0.293864    11.00000   -1.50000
H75B  2    0.623019    0.833293    0.249873    11.00000   -1.50000
H75C  2    0.586787    0.772452    0.245350    11.00000   -1.50000
AFIX   0
C260  1    0.939904    0.835863    0.273958    11.00000    0.02256    0.02875 =
         0.01904    0.00425    0.00781    0.00930
C360  1    1.048381    0.659207    0.424476    11.00000    0.02273    0.02089 =
         0.03226   -0.00037   -0.00288    0.00410
C65   1    0.659492    0.930213    0.568138    11.00000    0.03195    0.02179 =
         0.02189    0.00133   -0.00012    0.00732
C37   1    0.932181    0.575643    0.407443    11.00000    0.03097    0.01942 =
         0.02137   -0.00050    0.00144    0.00646
AFIX  43
H37   2    0.993606    0.555046    0.413022    11.00000   -1.20000
AFIX   0
C362  1    1.052562    0.685350    0.481808    11.00000    0.03368    0.02586 =
         0.03769   -0.00388   -0.00901    0.00158
AFIX 137
H36A  2    0.999427    0.713150    0.482561    11.00000   -1.50000
H36B  2    1.121263    0.701093    0.489949    11.00000   -1.50000
H36C  2    1.039601    0.658102    0.508649    11.00000   -1.50000
AFIX   0
C54   1    0.606422    0.598315    0.496741    11.00000    0.04506    0.02481 =
         0.02134   -0.00227    0.01013   -0.00503
AFIX  43
H54   2    0.640570    0.568052    0.483482    11.00000   -1.20000
AFIX   0
C32   1    0.585838    0.644518    0.329582    11.00000    0.03448    0.02596 =
         0.03359   -0.01229   -0.00870   -0.00350
AFIX  43
H32   2    0.588823    0.609941    0.314421    11.00000   -1.20000
AFIX   0
C55   1    0.666421    0.638984    0.523379    11.00000    0.03512    0.02660 =
         0.02009    0.00280    0.00682   -0.00858
C160  1    1.076409    0.891698    0.511698    11.00000    0.02358    0.02241 =
         0.03142   -0.00044   -0.00033   -0.00206
C17   1    1.019326    0.907008    0.608560    11.00000    0.02845    0.01824 =
         0.03037   -0.00751   -0.01265    0.00287
AFIX  43
H17   2    1.074645    0.931840    0.613099    11.00000   -1.20000
AFIX   0
C361  1    1.067979    0.702380    0.380759    11.00000    0.02336    0.03020 =
         0.04076    0.00355    0.00222    0.00213
AFIX 137
H36D  2    1.065838    0.685543    0.345289    11.00000   -1.50000
H36E  2    1.136238    0.718701    0.388649    11.00000   -1.50000
H36F  2    1.014084    0.729829    0.381067    11.00000   -1.50000
AFIX   0
C263  1    0.902986    0.777178    0.278041    11.00000    0.03453    0.02739 =
         0.01917   -0.00516    0.00217    0.00686
AFIX 137
H26A  2    0.881539    0.770344    0.314341    11.00000   -1.50000
H26B  2    0.960020    0.753174    0.270431    11.00000   -1.50000
H26C  2    0.844133    0.771029    0.251926    11.00000   -1.50000
AFIX   0
C262  1    1.028984    0.847435    0.318436    11.00000    0.02037    0.03097 =
         0.03338   -0.00209    0.00335    0.00145
AFIX 137
H26D  2    1.051990    0.884428    0.315475    11.00000   -1.50000
H26E  2    1.087527    0.823470    0.313594    11.00000   -1.50000
H26F  2    1.002977    0.841622    0.353973    11.00000   -1.50000
AFIX   0
C27   1    0.805932    0.906200    0.236634    11.00000    0.02696    0.02444 =
         0.01579    0.00139    0.00466    0.00239
AFIX  43
H27   2    0.837762    0.903293    0.203546    11.00000   -1.20000
AFIX   0
C74   1    0.455611    0.861418    0.296456    11.00000    0.02831    0.02714 =
         0.02717    0.00088    0.00174   -0.00577
AFIX  43
H74   2    0.477816    0.887385    0.272074    11.00000   -1.20000
AFIX   0
C18   1    0.956494    0.897940    0.652626    11.00000    0.03973    0.01982 =
         0.02317   -0.00642   -0.00903    0.00637
C61   1    0.499633    0.885523    0.528871    11.00000    0.02435    0.02003 =
         0.02652   -0.00247    0.00806    0.00421
C39   1    0.747235    0.580412    0.384168    11.00000    0.03391    0.01665 =
         0.01807   -0.00170    0.00224   -0.00299
AFIX  43
H39   2    0.682440    0.563787    0.374980    11.00000   -1.20000
AFIX   0
C161  1    1.122836    0.838103    0.490701    11.00000    0.02616    0.03076 =
         0.03955   -0.00241    0.00621   -0.00076
AFIX 137
H16A  2    1.161126    0.819750    0.520469    11.00000   -1.50000
H16B  2    1.169955    0.845990    0.462531    11.00000   -1.50000
H16C  2    1.066269    0.815275    0.476059    11.00000   -1.50000
AFIX   0
C72   1    0.333018    0.832087    0.360070    11.00000    0.01787    0.04203 =
         0.02909   -0.00491   -0.00013    0.00275
AFIX  43
H72   2    0.271021    0.837717    0.377717    11.00000   -1.20000
AFIX   0
C28   1    0.720050    0.942010    0.239358    11.00000    0.02585    0.02057 =
         0.01876    0.00254    0.00156    0.00207
C162  1    1.014187    0.921361    0.463751    11.00000    0.03360    0.02437 =
         0.03374    0.00230   -0.00137   -0.00416
AFIX 137
H16D  2    0.957265    0.898624    0.449358    11.00000   -1.50000
H16E  2    1.060968    0.929074    0.435382    11.00000   -1.50000
H16F  2    0.985808    0.954751    0.476829    11.00000   -1.50000
AFIX   0
C53   1    0.496515    0.601833    0.489459    11.00000    0.03904    0.02815 =
         0.01963    0.00236    0.00260   -0.01218
C71   1    0.389635    0.785015    0.370718    11.00000    0.02014    0.03317 =
         0.02190    0.00125   -0.00125   -0.00660
C64   1    0.625859    0.917939    0.619984    11.00000    0.05557    0.03277 =
         0.01790   -0.00165    0.00048    0.01164
AFIX  43
H64   2    0.667861    0.928742    0.650724    11.00000   -1.20000
AFIX   0
C50   1    0.612702    0.683697    0.541942    11.00000    0.04446    0.02359 =
         0.01869   -0.00087    0.01097   -0.01333
C33   1    0.511228    0.681669    0.318193    11.00000    0.03478    0.03039 =
         0.03455   -0.01068   -0.00982   -0.00058
AFIX  43
H33   2    0.452184    0.677988    0.293709    11.00000   -1.20000
AFIX   0
C650  1    0.758898    0.962101    0.561459    11.00000    0.03170    0.03032 =
         0.03296   -0.00006   -0.00830    0.00046
AFIX 137
H65A  2    0.790530    0.950496    0.528801    11.00000   -1.50000
H65B  2    0.807741    0.956139    0.592630    11.00000   -1.50000
H65C  2    0.742041    1.000074    0.558670    11.00000   -1.50000
AFIX   0
C51   1    0.502909    0.687934    0.537059    11.00000    0.04304    0.02399 =
         0.02865    0.00323    0.01457   -0.00404
C62   1    0.470384    0.874787    0.581562    11.00000    0.03800    0.02479 =
         0.03845    0.00308    0.02052    0.00389
AFIX  43
H62   2    0.407133    0.856592    0.586163    11.00000   -1.20000
AFIX   0
C52   1    0.446575    0.646325    0.510582    11.00000    0.03221    0.02883 =
         0.03086    0.00584    0.00552   -0.00764
AFIX  43
H52   2    0.373013    0.648370    0.506904    11.00000   -1.20000
AFIX   0
C73   1    0.364978    0.871383    0.324039    11.00000    0.02182    0.03165 =
         0.03477   -0.00352   -0.00632    0.00027
C610  1    0.431167    0.868560    0.479318    11.00000    0.02785    0.03417 =
         0.04866   -0.00452    0.00414   -0.00550
AFIX 137
H61A  2    0.415303    0.899674    0.456556    11.00000   -1.50000
H61B  2    0.366416    0.853164    0.490692    11.00000   -1.50000
H61C  2    0.467993    0.841992    0.459012    11.00000   -1.50000
AFIX   0
C163  1    1.170762    0.927188    0.531040    11.00000    0.02762    0.02988 =
         0.04692   -0.00216   -0.00255   -0.00924
AFIX 137
H16G  2    1.145985    0.962591    0.540592    11.00000   -1.50000
H16H  2    1.218222    0.930441    0.502157    11.00000   -1.50000
H16I  2    1.207349    0.910827    0.562522    11.00000   -1.50000
AFIX   0

C1S   1    0.145503    0.740435    0.620717    11.00000    0.04631    0.03452 =
         0.03267    0.00605    0.00132   -0.00257
AFIX  43
H1S   2    0.099510    0.743605    0.589593    11.00000   -1.20000
AFIX   0

C261  1    0.988294    0.843471    0.218319    11.00000    0.03459    0.05163 =
         0.02930    0.00687    0.01589    0.02042
AFIX 137
H26G  2    0.937109    0.833453    0.189324    11.00000   -1.50000
H26H  2    1.049929    0.820878    0.216871    11.00000   -1.50000
H26I  2    1.008015    0.880825    0.214073    11.00000   -1.50000
AFIX   0
C280  1    0.672145    0.971999    0.188677    11.00000    0.03613    0.02836 =
         0.01658    0.00226    0.00047    0.00999
C363  1    1.140776    0.618447    0.423836    11.00000    0.02435    0.02788 =
         0.05902   -0.00147   -0.00677    0.00788
AFIX 137
H36G  2    1.135683    0.592731    0.453065    11.00000   -1.50000
H36H  2    1.206855    0.637612    0.428656    11.00000   -1.50000
H36I  2    1.137354    0.599602    0.389390    11.00000   -1.50000
AFIX   0
C38   1    0.836734    0.548359    0.395390    11.00000    0.03615    0.01736 =
         0.01859    0.00098    0.00219   -0.00158
C710  1    0.356883    0.743667    0.411303    11.00000    0.02826    0.04677 =
         0.03298    0.00487    0.00873   -0.00718
AFIX 137
H71A  2    0.334220    0.711116    0.392328    11.00000   -1.50000
H71B  2    0.299575    0.757865    0.430848    11.00000   -1.50000
H71C  2    0.415875    0.735537    0.436728    11.00000   -1.50000
AFIX   0
C380  1    0.828785    0.486024    0.393570    11.00000    0.04440    0.01989 =
         0.03309    0.00043    0.00135   -0.00092
C180  1    0.978460    0.928903    0.706951    11.00000    0.05757    0.03184 =
         0.02777   -0.01289   -0.01314    0.00804
C510  1    0.447102    0.736280    0.560156    11.00000    0.05906    0.02829 =
         0.05506   -0.00102    0.02224    0.00250
AFIX 137
H51A  2    0.450037    0.733703    0.599401    11.00000   -1.50000
H51B  2    0.374449    0.736704    0.546019    11.00000   -1.50000
H51C  2    0.481382    0.769134    0.549713    11.00000   -1.50000
AFIX   0
C550  1    0.784579    0.633540    0.532246    11.00000    0.04087    0.04153 =
         0.03071    0.00266    0.00303   -0.00865
AFIX 137
H55A  2    0.803506    0.628750    0.570613    11.00000   -1.50000
H55B  2    0.817901    0.665760    0.519459    11.00000   -1.50000
H55C  2    0.807874    0.602630    0.512334    11.00000   -1.50000
AFIX   0
C63   1    0.533124    0.890518    0.627411    11.00000    0.05239    0.03664 =
         0.02388    0.00528    0.01482    0.01134

C3S   1    0.279018    0.690866    0.674078    11.00000    0.03933    0.03072 =
         0.05955    0.00843    0.00072    0.00669
AFIX  43
H3S   2    0.323157    0.660728    0.678335    11.00000   -1.20000
AFIX   0
C2S   1    0.211283    0.696445    0.627283    11.00000    0.04828    0.03489 =
         0.04151   -0.00419    0.00920   -0.00301
AFIX  43
H2S   2    0.210664    0.669974    0.600123    11.00000   -1.20000
AFIX   0

C283  1    0.756129    0.984881    0.149154    11.00000    0.05358    0.05270 =
         0.03280    0.02550    0.00335    0.00721
AFIX 137
H28A  2    0.814531    1.003068    0.168419    11.00000   -1.50000
H28B  2    0.726448    1.007981    0.120457    11.00000   -1.50000
H28C  2    0.780586    0.951749    0.133559    11.00000   -1.50000
AFIX   0

C4S   1    0.280296    0.729846    0.713653    11.00000    0.04493    0.03669 =
         0.05662    0.00811   -0.01804    0.00229
AFIX  43
H4S   2    0.325287    0.726201    0.745095    11.00000   -1.20000
AFIX   0

C183  1    0.970374    0.989760    0.697387    11.00000    0.09819    0.03626 =
         0.04178   -0.01933    0.00344   -0.00739
AFIX 137
H18A  2    1.016631    1.000131    0.669602    11.00000   -1.50000
H18B  2    0.990692    1.008583    0.730832    11.00000   -1.50000
H18C  2    0.898685    0.999043    0.685679    11.00000   -1.50000
AFIX   0
C12   1    0.763974    0.760504    0.641483    11.00000    0.09878    0.03953 =
         0.01756    0.00729   -0.00415   -0.03149
AFIX  43
H12   2    0.792657    0.768344    0.676601    11.00000   -1.20000
AFIX   0
C13   1    0.698512    0.720506    0.627588    11.00000    0.11696    0.04684 =
         0.01335    0.00306    0.00692   -0.04406
AFIX  43
H13   2    0.673411    0.694315    0.650890    11.00000   -1.20000
AFIX   0
C530  1    0.433589    0.559340    0.457881    11.00000    0.04926    0.04214 =
         0.03681   -0.00662   -0.00316   -0.01498
AFIX 137
H53A  2    0.412038    0.573056    0.422112    11.00000   -1.50000
H53B  2    0.371995    0.550246    0.476920    11.00000   -1.50000
H53C  2    0.476388    0.527474    0.454363    11.00000   -1.50000
AFIX   0
C730  1    0.303726    0.923555    0.315109    11.00000    0.04247    0.04173 =
         0.06278    0.00541   -0.00195    0.01397
AFIX 137
H73A  2    0.352228    0.953549    0.314893    11.00000   -1.50000
H73B  2    0.257052    0.928378    0.344131    11.00000   -1.50000
H73C  2    0.262905    0.921951    0.280619    11.00000   -1.50000
AFIX   0

C6S   1    0.148065    0.780165    0.660831    11.00000    0.07196    0.03568 =
         0.05683    0.00022   -0.02033    0.01921
AFIX  43
H6S   2    0.104665    0.810583    0.656583    11.00000   -1.20000
AFIX   0
C5S   1    0.215831    0.774284    0.707413    11.00000    0.07263    0.04339 =
         0.06040   -0.01367   -0.02567    0.01459
AFIX  43
H5S   2    0.217415    0.800762    0.734589    11.00000   -1.20000
AFIX   0

C630  1    0.500009    0.877253    0.684233    11.00000    0.09290    0.05865 =
         0.03349    0.00890    0.02714    0.00539
AFIX 137
H63A  2    0.543964    0.848626    0.699763    11.00000   -1.50000
H63B  2    0.427313    0.865749    0.681986    11.00000   -1.50000
H63C  2    0.507739    0.908970    0.707000    11.00000   -1.50000
AFIX   0
C281  1    0.590860    0.935911    0.158241    11.00000    0.06072    0.07893 =
         0.05089    0.03726   -0.03444   -0.02853
AFIX 137
H28D  2    0.623800    0.902459    0.148474    11.00000   -1.50000
H28E  2    0.563142    0.954077    0.125629    11.00000   -1.50000
H28F  2    0.534161    0.928345    0.181344    11.00000   -1.50000
AFIX   0
C181  1    0.900168    0.912590    0.749421    11.00000    0.14400    0.05695 =
         0.02396   -0.01993    0.00908   -0.02245
AFIX 137
H18D  2    0.829924    0.923630    0.736816    11.00000   -1.50000
H18E  2    0.919745    0.930050    0.783715    11.00000   -1.50000
H18F  2    0.901870    0.873889    0.754295    11.00000   -1.50000
AFIX   0
PART 1
C381  1    0.786961    0.467864    0.335412    21.00000    0.06370    0.01651 =
         0.04721   -0.00777    0.00809   -0.00828
AFIX 137
H38A  2    0.834162    0.480568    0.309019    21.00000   -1.50000
H38B  2    0.717647    0.482850    0.327162    21.00000   -1.50000
H38C  2    0.783168    0.428927    0.334032    21.00000   -1.50000
AFIX   0
C383  1    0.757168    0.465644    0.434624    21.00000    0.05984    0.01688 =
         0.04769    0.00258    0.01696    0.00179
AFIX 137
H38D  2    0.754030    0.426704    0.432908    21.00000   -1.50000
H38E  2    0.687468    0.480362    0.426914    21.00000   -1.50000
H38F  2    0.783654    0.476676    0.470621    21.00000   -1.50000
AFIX   0
PART 0
C182  1    1.089648    0.913570    0.731102    11.00000    0.10916    0.13613 =
         0.07032   -0.07126   -0.06550    0.06297
AFIX 137
H18G  2    1.095579    0.874739    0.733422    11.00000   -1.50000
H18H  2    1.101064    0.929002    0.767066    11.00000   -1.50000
H18I  2    1.141809    0.927382    0.707918    11.00000   -1.50000
AFIX   0
C282  1    0.621626    1.025079    0.204501    11.00000    0.15968    0.08194 =
         0.02736    0.01654    0.01027    0.08789
AFIX 137
H28G  2    0.562750    1.017690    0.226210    11.00000   -1.50000
H28H  2    0.597208    1.044402    0.171972    11.00000   -1.50000
H28I  2    0.672923    1.046767    0.225342    11.00000   -1.50000
AFIX   0
PART 1
C385  1    0.940255    0.457649    0.404285    21.00000    0.04490    0.02030 =
         0.07667   -0.00137    0.00759    0.00369
AFIX 137
H38G  2    0.931022    0.418944    0.404946    21.00000   -1.50000
H38H  2    0.972498    0.469565    0.438866    21.00000   -1.50000
H38I  2    0.985002    0.467191    0.375554    21.00000   -1.50000
AFIX   0
PART 0
PART 2
C386  1    0.888564    0.463092    0.357011   -21.00000    0.07260    0.02188 =
         0.06031   -0.00293    0.05172    0.00577
AFIX 137
H38J  2    0.900048    0.425546    0.366243   -21.00000   -1.50000
H38K  2    0.955508    0.481522    0.357328   -21.00000   -1.50000
H38L  2    0.853165    0.465701    0.321145   -21.00000   -1.50000
AFIX   0
C382  1    0.707148    0.469007    0.384720   -21.00000    0.05984    0.01688 =
         0.04769    0.00258    0.01696    0.00179
AFIX 137
H38M  2    0.682296    0.476074    0.347450   -21.00000   -1.50000
H38N  2    0.666066    0.489713    0.408955   -21.00000   -1.50000
H38O  2    0.699875    0.430993    0.392427   -21.00000   -1.50000
AFIX   0
C384  1    0.852508    0.467174    0.454699   -21.00000    0.05241    0.00977 =
         0.03564   -0.00098   -0.00818   -0.00157
AFIX 137
H38P  2    0.843529    0.428532    0.457071   -21.00000   -1.50000
H38Q  2    0.804423    0.484921    0.477680   -21.00000   -1.50000
H38R  2    0.924034    0.476577    0.466610   -21.00000   -1.50000
AFIX   0
HKLF 4

REM  p17079_a.res in P2(1)/c
REM R1 =  0.0459 for   13869 Fo > 4sig(Fo)  and  0.0742 for all   18512 data
REM    899 parameters refined using      0 restraints

END  
     
WGHT      0.0351      6.7793 

REM Highest difference peak  0.883,  deepest hole -0.450,  1-sigma level  0.085
Q1    1   0.7550  0.7884  0.3998  11.00000  0.05    0.88
Q2    1   0.7585  0.7963  0.4811  11.00000  0.05    0.78
Q3    1   0.7474  0.7564  0.4389  11.00000  0.05    0.48
Q4    1   0.8913  0.8607  0.2786  11.00000  0.05    0.43
Q5    1   0.7628  0.6206  0.4399  11.00000  0.05    0.42
Q6    1   1.0556  0.9001  0.4802  11.00000  0.05    0.40
Q7    1   1.0033  0.9009  0.5810  11.00000  0.05    0.38
Q8    1   0.7025  0.9599  0.2164  11.00000  0.05    0.37
Q9    1   0.8434  0.8973  0.2632  11.00000  0.05    0.36
Q10   1   0.6670  0.8615  0.4408  11.00000  0.05    0.36
Q11   1   1.1015  0.6396  0.4199  11.00000  0.05    0.35
Q12   1   0.6868  0.9428  0.2519  11.00000  0.05    0.34
Q13   1   0.6775  0.9194  0.3600  11.00000  0.05    0.33
Q14   1   0.1768  0.7611  0.6368  11.00000  0.05    0.33
Q15   1   0.4999  0.8398  0.3012  11.00000  0.05    0.33
Q16   1   0.4709  0.8779  0.5013  11.00000  0.05    0.33
Q17   1   0.3235  0.9402  0.2811  11.00000  0.05    0.33
Q18   1   0.4197  0.8615  0.3195  11.00000  0.05    0.32
Q19   1   0.6363  0.6194  0.5197  11.00000  0.05    0.32
Q20   1   0.5459  0.9032  0.5176  11.00000  0.05    0.31

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0459 for 13869 Fo > 4sig(Fo) and 0.0742 for all 81858 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.88, deepest hole -0.45
  REM Mean Shift 0, Max Shift -0.004.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0742
  REM R1_gt = 0.0459
  REM wR_ref = 0.1419
  REM GOOF = 0.916
  REM Shift_max = -0.004
  REM Shift_mean = 0
  REM Reflections_all = 81858
  REM Reflections_gt = 13869
  REM Parameters = n/a
  REM Hole = -0.45
  REM Peak = 0.88
  REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.112
_oxdiff_exptl_absorpt_empirical_full_min 0.887