Carbon Chain Growth by Sequential Reactions of CO and CO<sub>2</sub> with [W(CO)<sub>6</sub>] and an Aluminum(I) Reductant.
Kong, Richard Y.; Crimmin, Mark R.; Journal of the American Chemical Society 140 (2018) 13614–13617; doi:10.1021/jacs.8b09761

data_4133377
_publ_section_title
;
 Carbon Chain Growth by Sequential Reactions of CO and CO<sub>2</sub> with
 [W(CO)<sub>6</sub>] and an Aluminum(I) Reductant.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13614
_journal_page_last               13617
_journal_paper_doi               10.1021/jacs.8b09761
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C67 H82 Al2 N4 O9 W, C7 H8'
_chemical_formula_sum            'C74 H90 Al2 N4 O9 W'
_chemical_formula_weight         1417.30
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.4806(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3318(3)
_cell_length_b                   21.4894(3)
_cell_length_c                   21.5498(3)
_cell_measurement_reflns_used    7947
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      73.5810
_cell_measurement_theta_min      4.0060
_cell_volume                     7093.4(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.955
_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    -51.00  31.00   1.00    2.42    --  -41.86  57.00-120.00   82
  2  \w    -60.00  26.00   1.00    2.42    --  -41.86  38.00 150.00   86
  3  \w     79.00 175.00   1.00    8.89    --  106.38  61.00-150.00   96
  4  \w     46.00 135.00   1.00    8.89    --  106.38 -30.00  30.00   89
  5  \w     34.00 116.00   1.00    8.89    --  106.38-125.00 -60.00   82
  6  \w     26.00 109.00   1.00    8.89    --  106.38 -95.00 -30.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0955917000
_diffrn_orient_matrix_UB_12      -0.0218268000
_diffrn_orient_matrix_UB_13      0.0004006000
_diffrn_orient_matrix_UB_21      -0.0246509000
_diffrn_orient_matrix_UB_22      0.0470591000
_diffrn_orient_matrix_UB_23      -0.0517992000
_diffrn_orient_matrix_UB_31      0.0186888000
_diffrn_orient_matrix_UB_32      -0.0494718000
_diffrn_orient_matrix_UB_33      -0.0494820000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23112
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.707
_diffrn_reflns_theta_min         3.544
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.715
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.354
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       plate
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.274
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         13687
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10456
_reflns_number_total             13687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09761_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        7093.40(18)
_cod_database_code               4133377
_shelx_shelxl_version_number     2016/6
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C125 H164 Al4 N8 O9 W'
_reflns_odcompleteness_completeness 98.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
C69 \\sim C71 \\sim C68 \\sim C74 \\sim C73 \\sim C72 \\sim C70 \\sim C168
\\sim C169 \\sim C170 \\sim C171 \\sim C174 \\sim C172 \\sim C173: within 1A
with sigma of 0 and sigma for terminal atoms of 0.01
3. Others
 Sof(C168)=Sof(C169)=Sof(H169)=Sof(C170)=Sof(H170)=Sof(C171)=Sof(H171)=
 Sof(C172)=Sof(H172)=Sof(C173)=Sof(H173)=Sof(C174)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=1-FVAR(1)
 Sof(C68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71)=Sof(C72)=
 Sof(H72)=Sof(C73)=Sof(H73)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C65(H65), C50(H50), C62(H62), C21(H21), C36(H36), C24(H24), C33(H33), C53(H53)
4.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C29(H29), C30(H30), C48(H48), C46(H46), C47(H47), C60(H60),
 C58(H58), C31(H31), C59(H59), C19(H19), C12(H12), C18(H18), C69(H69), C70(H70),
  C71(H71), C72(H72), C73(H73), C17(H17), C169(H169), C170(H170), C171(H171),
 C172(H172), C173(H173)
4.c Fitted hexagon refined as free rotating group:
 C68(C69,C70,C71,C72,C73), C168(C169,C170,C171,C172,C173)
4.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C43(H43A,H43B,H43C), C67(H67A,H67B,H67C), C66(H66A,H66B,
 H66C), C51(H51A,H51B,H51C), C64(H64A,H64B,H64C), C37(H37A,H37B,H37C), C63(H63A,
 H63B,H63C), C25(H25A,H25B,H25C), C54(H54A,H54B,H54C), C52(H52A,H52B,H52C),
 C26(H26A,H26B,H26C), C55(H55A,H55B,H55C), C14(H14A,H14B,H14C), C23(H23A,H23B,
 H23C), C39(H39A,H39B,H39C), C74(H74A,H74B,H74C), C38(H38A,H38B,H38C), C35(H35A,
 H35B,H35C), C34(H34A,H34B,H34C), C22(H22A,H22B,H22C), C174(H17A,H17B,H17C)
;
_ins_header
;
TITL MRC1835 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  15.331795  21.489410  21.549840  90.0000  92.4806  90.0000
ZERR    3.00   0.000259   0.000274   0.000307   0.0000   0.0014   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O Al W
UNIT 375.00 492.00 24.00 27.00 12.00 3.00
TREF
HKLF 4
END
;
_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 1.192
_oxdiff_exptl_absorpt_empirical_full_min 0.813