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_4133376
_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         'C66 H82 Al2 N4 O8 W, 3.5(C7 H8)'
_chemical_formula_sum            'C90.5 H110 Al2 N4 O8 W'
_chemical_formula_weight         1619.63
_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     dual
_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                 102.219(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.7428(6)
_cell_length_b                   12.2385(2)
_cell_length_c                   25.2788(5)
_cell_measurement_reflns_used    7446
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      28.0310
_cell_measurement_theta_min      2.5480
_cell_volume                     8388.5(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      173.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.803
_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     -1.00  79.00   1.00    8.55    --   14.27  57.00  60.00   80
  2  \w     -6.00  74.00   1.00    8.55    --   14.27  77.00 150.00   80
;
_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      -0.0259052000
_diffrn_orient_matrix_UB_12      -0.0018695000
_diffrn_orient_matrix_UB_13      -0.0098783000
_diffrn_orient_matrix_UB_21      -0.0033321000
_diffrn_orient_matrix_UB_22      -0.0131503000
_diffrn_orient_matrix_UB_23      0.0263210000
_diffrn_orient_matrix_UB_31      -0.0016423000
_diffrn_orient_matrix_UB_32      0.0563932000
_diffrn_orient_matrix_UB_33      0.0057997000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.803
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28236
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         2.454
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.385
_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    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             3380
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.378
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         16764
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0265P)^2^+3.1481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12954
_reflns_number_total             16764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09761_si_002.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C90.50 H110 Al2 N4 O8 W'
_cod_database_code               4133376
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C34 H41 Al N2 O5 W'
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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. Uiso/Uaniso restraints and constraints
C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C74 \\sim C80 \\sim C174
\\sim C179 \\sim C178 \\sim C177 \\sim C176 \\sim C175 \\sim C180: within 1A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C67 \\sim C73 \\sim C167
\\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim C173 \\sim C172: within 1A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C128 \\sim C129 \\sim C28 \\sim C29: within 1A with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Others
 Sof(C174)=Sof(C179)=Sof(H179)=Sof(C178)=Sof(H178)=Sof(C177)=Sof(H177)=
 Sof(C176)=Sof(H176)=Sof(C175)=Sof(H175)=Sof(C180)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=1-FVAR(1)
 Sof(C75)=Sof(H75)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77)=Sof(C78)=Sof(H78)=
 Sof(C79)=Sof(H79)=Sof(C74)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=FVAR(1)
 Sof(C167)=Sof(C168)=Sof(H168)=Sof(C169)=Sof(H169)=Sof(C170)=Sof(H170)=
 Sof(C171)=Sof(H171)=Sof(C172)=Sof(H172)=Sof(C173)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=1-FVAR(2)
 Sof(C68)=Sof(H68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71)=
 Sof(C72)=Sof(H72)=Sof(C67)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=FVAR(2)
 Sof(H27A)=Sof(C129)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C128)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=1-FVAR(3)
 Sof(H27)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=FVAR(3)
 Fixed Sof: C89(0.5) H89(0.5) C88(0.5) C93(0.5) H93(0.5) C92(0.5) H92(0.5)
 C91(0.5) H91(0.5) C90(0.5) H90(0.5) C94(0.5) H94A(0.5) H94B(0.5) H94C(0.5)
4.a Ternary CH refined with riding coordinates:
 C30(H30), C15(H15), C18(H18), C47(H47), C27(H27), C27(H27A), C44(H44),
 C59(H59), C56(H56)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C35(H35), C12(H12), C13(H13), C23(H23), C6(H6), C25(H25), C24(H24),
 C40(H40), C42(H42), C52(H52), C54(H54), C41(H41), C53(H53), C89(H89), C93(H93),
  C92(H92), C91(H91), C90(H90), C68(H68), C69(H69), C70(H70), C71(H71),
 C72(H72), C83(H83), C82(H82), C86(H86), C85(H85), C84(H84), C75(H75), C76(H76),
  C77(H77), C78(H78), C79(H79), C179(H179), C178(H178), C177(H177), C176(H176),
 C175(H175), C168(H168), C169(H169), C170(H170), C171(H171), C172(H172)
4.c Fitted hexagon refined as free rotating group:
 C89(C88,C93,C92,C91,C90), C68(C69,C70,C71,C72,C67), C75(C76,C77,C78,C79,C74),
 C174(C179,C178,C177,C176,C175), C167(C168,C169,C170,C171,C172)
4.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C16(H16A,H16B,H16C), C4(H4A,H4B,
 H4C), C61(H61A,H61B,H61C), C31(H31A,H31B,H31C), C17(H17A,H17B,H17C), C49(H49A,
 H49B,H49C), C37(H37A,H37B,H37C), C48(H48A,H48B,H48C), C8(H8A,H8B,H8C),
 C19(H19A,H19B,H19C), C58(H58A,H58B,H58C), C20(H20A,H20B,H20C), C45(H45A,H45B,
 H45C), C60(H60A,H60B,H60C), C46(H46A,H46B,H46C), C57(H57A,H57B,H57C), C29(H29A,
 H29B,H29C), C28(H28A,H28B,H28C), C94(H94A,H94B,H94C), C73(H73A,H73B,H73C),
 C87(H87A,H87B,H87C), C80(H80A,H80B,H80C), C180(H18A,H18B,H18C), C173(H17D,H17E,
 H17F), C129(H12A,H12B,H12C), C128(H12D,H12E,H12F)
;
_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 1.087
_oxdiff_exptl_absorpt_empirical_full_min 0.884