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_4133379
_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 O10 W, 1.5(C7 H8)'
_chemical_formula_sum            'C77.5 H94 Al2 N4 O10 W'
_chemical_formula_weight         1479.37
_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             2018-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.273(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.7014(9)
_cell_length_b                   15.0966(4)
_cell_length_c                   28.7796(9)
_cell_measurement_reflns_used    11217
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      73.4030
_cell_measurement_theta_min      3.8360
_cell_volume                     14859.3(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.976
_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    -13.00  82.00   1.00   17.55    --   41.86 -99.00  90.00   95
  2  \w    -30.00  48.00   1.00   17.55    --   41.86 -38.00-180.00   78
  3  \w     74.00 167.00   1.00   93.04    --  106.38  77.00 -90.00   93
  4  \w     35.00 128.00   1.00   93.04    --  106.38 -45.00 120.00   93
  5  \w     24.00 109.00   1.00   93.04    --  106.38 -95.00 -30.00   85
  6  \w     84.00 175.00   1.00   93.04    --  106.38  30.00   0.00   91
;
_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      -0.0046166000
_diffrn_orient_matrix_UB_12      -0.0722706000
_diffrn_orient_matrix_UB_13      0.0353162000
_diffrn_orient_matrix_UB_21      -0.0445397000
_diffrn_orient_matrix_UB_22      -0.0003881000
_diffrn_orient_matrix_UB_23      -0.0285389000
_diffrn_orient_matrix_UB_31      0.0048044000
_diffrn_orient_matrix_UB_32      -0.0719938000
_diffrn_orient_matrix_UB_33      -0.0351845000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.1056
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            33683
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.898
_diffrn_reflns_theta_min         3.296
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.580
_exptl_absorpt_correction_T_max  -0.010
_exptl_absorpt_correction_T_min  10000000.000
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             6136
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.824
_refine_diff_density_min         -1.482
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1825
_refine_ls_number_reflns         33683
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0710
_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^)+(0.0517P)^2^+116.0649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23300
_reflns_number_total             33683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09761_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        14859.2(8)
_cod_original_formula_sum        'C77.50 H94 Al2 N4 O10 W'
_cod_database_code               4133379
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C66 H40 O11 N4 Al2 W'
_chemical_oxdiff_usercomment     RK119
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.485
_reflns_odcompleteness_completeness 97.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7051(8)
 0.2949(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C90-C96
 1.4 with sigma of 0.02
 C89-C83
 1.4 with sigma of 0.02
 C92-C93 \\sim C91-C90
 with sigma of 0.02
 C92-C94 \\sim C91-C95
 with sigma of 0.02
 C93-C94 \\sim C90-C95
 with sigma of 0.04
 C91-C96 \\sim C96-C95
 with sigma of 0.02
 C88-C89 \\sim C89-C84
 with sigma of 0.02
 C65-C66 \\sim C65-C67
 with sigma of 0.02
 C65A-C66A \\sim C65A-C67A
 with sigma of 0.02
 C65A-C61 \\sim C61-C65
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C92 \\sim C91 \\sim C90 \\sim C95 \\sim C94 \\sim C93 \\sim C96: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C87 \\sim C86 \\sim C85 \\sim C84 \\sim C83 \\sim C88 \\sim C89: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C134 \\sim C133 \\sim C135: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
C67 \\sim C65 \\sim C67A \\sim C65A \\sim C66A \\sim C66: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.01
C233 \\sim C234 \\sim C235 \\sim C133 \\sim C135 \\sim C134 \\sim C128: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.01
5. Others
 Sof(C133)=Sof(H133)=Sof(C135)=Sof(H13J)=Sof(H13K)=Sof(H13L)=Sof(C134)=
 Sof(H13M)=Sof(H13N)=Sof(H13O)=1-FVAR(1)
 Sof(C233)=Sof(H233)=Sof(C234)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C235)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=FVAR(1)
 Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C65A)=Sof(H65A)=Sof(C66A)=
 Sof(H66D)=Sof(H66E)=Sof(H66F)=1-FVAR(2)
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=
 Sof(C65)=Sof(H65)=FVAR(2)
 Fixed Sof: C92(0.5) H92(0.5) C91(0.5) H91(0.5) C90(0.5) C95(0.5) H95(0.5)
 C94(0.5) H94(0.5) C93(0.5) H93(0.5) C87(0.5) H87(0.5) C86(0.5) H86(0.5)
 C85(0.5) H85(0.5) C84(0.5) H84(0.5) C83(0.5) C88(0.5) H88(0.5) C89(0.5)
 H89A(0.5) H89B(0.5) H89C(0.5) C96(0.5) H96A(0.5) H96B(0.5) H96C(0.5)
6.a Ternary CH refined with riding coordinates:
 C124(H124), C153(H153), C53(H53), C21(H21), C150(H150), C24(H24), C136(H136),
 C162(H162), C50(H50), C33(H33), C121(H121), C62(H62), C36(H36), C165(H165),
 C233(H233), C65(H65), C133(H133), C65A(H65A)
6.b Me refined with riding coordinates:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C234(H23A,H23B,H23C), C235(H23D,
 H23E,H23F), C89(H89A,H89B,H89C), C135(H13J,H13K,H13L), C134(H13M,H13N,H13O),
 C67A(H67D,H67E,H67F), C66A(H66D,H66E,H66F)
6.c Aromatic/amide H refined with riding coordinates:
 C141(H141), C41(H41), C117(H117), C18(H18), C19(H19), C31(H31), C58(H58),
 C74(H74), C158(H158), C59(H59), C146(H146), C131(H131), C160(H160), C12(H12),
 C129(H129), C46(H46), C47(H47), C112(H112), C118(H118), C119(H119), C60(H60),
 C48(H48), C81(H81), C80(H80), C79(H79), C78(H78), C77(H77), C148(H148),
 C147(H147), C159(H159), C29(H29), C73(H73), C70(H70), C69(H69), C71(H71),
 C130(H130), C17(H17), C30(H30), C92(H92), C91(H91), C95(H95), C94(H94),
 C93(H93), C87(H87), C86(H86), C85(H85), C84(H84), C88(H88)
6.d Fitted hexagon refined as free rotating group:
 C76(C81,C80,C79,C78,C77), C92(C91,C90,C95,C94,C93), C87(C86,C85,C84,C83,C88)
6.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C139(H13A,H13B,H13C), C154(H15A,H15B,H15C), C122(H12A,
 H12B,H12C), C155(H15D,H15E,H15F), C163(H16A,H16B,H16C), C25(H25A,H25B,H25C),
 C14(H14D,H14E,H14F), C54(H54A,H54B,H54C), C110(H11A,H11B,H11C), C151(H15G,H15H,
 H15I), C22(H22A,H22B,H22C), C137(H13D,H13E,H13F), C39(H39A,H39B,H39C),
 C152(H15J,H15K,H15L), C164(H16D,H16E,H16F), C51(H51A,H51B,H51C), C123(H12D,
 H12E,H12F), C64(H64A,H64B,H64C), C43(H43A,H43B,H43C), C63(H63A,H63B,H63C),
 C55(H55A,H55B,H55C), C26(H26A,H26B,H26C), C138(H13G,H13H,H13I), C34(H34A,H34B,
 H34C), C23(H23G,H23H,H23I), C75(H75A,H75B,H75C), C52(H52A,H52B,H52C),
 C114(H11D,H11E,H11F), C125(H12G,H12H,H12I), C82(H82A,H82B,H82C), C126(H12J,
 H12K,H12L), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C),
 C166(H16G,H16H,H16I), C167(H16J,H16K,H16L), C143(H14A,H14B,H14C), C96(H96A,
 H96B,H96C)
;
_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 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.843
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.9932\% 
 around [-0.42 0.00 0.91] (reciprocal) or [0.00 -0.00 1.00] (direct)
;