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_4133378
_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, 2(C6 H6)'
_chemical_formula_sum            'C79 H94 Al2 N4 O10 W'
_chemical_formula_weight         1497.39
_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             2018-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.815(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8441(9)
_cell_length_b                   19.0576(5)
_cell_length_c                   22.2871(8)
_cell_measurement_reflns_used    8462
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.3180
_cell_measurement_theta_min      3.8720
_cell_volume                     7569.9(5)
_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(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.974
_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    -89.00  -7.00   1.00    1.63    --  -41.86 125.00-120.00   82
  2  \w   -114.00 -23.00   1.00    1.63    --  -41.86 -57.00 120.00   91
  3  \w     65.00 131.00   1.00    6.99    --  106.38 -45.00  60.00   66
  4  \w     74.00 147.00   1.00    6.99    --  106.38  77.00-120.00   73
  5  \w     90.00 163.00   1.00    6.99    --  106.38  45.00-180.00   73
  6  \w     99.00 178.00   1.00    6.99    --  106.38 125.00  60.00   79
  7  \w     27.00 109.00   1.00    6.99    --  106.38 -95.00 120.00   82
;
_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      -0.0084062000
_diffrn_orient_matrix_UB_12      0.0794223000
_diffrn_orient_matrix_UB_13      0.0106110000
_diffrn_orient_matrix_UB_21      -0.0194837000
_diffrn_orient_matrix_UB_22      -0.0142699000
_diffrn_orient_matrix_UB_23      0.0654511000
_diffrn_orient_matrix_UB_31      0.0838915000
_diffrn_orient_matrix_UB_32      0.0046369000
_diffrn_orient_matrix_UB_33      0.0197538000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19606
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.790
_diffrn_reflns_theta_min         3.395
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.521
_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    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.491
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         19606
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0966P)^2^+1.8643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15819
_reflns_number_total             19606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09761_si_002.cif
_cod_data_source_block           4
_cod_database_code               4133378
_shelx_shelxl_version_number     2016/6
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C66 H82 N4 O8 Al2 W'
_chemical_oxdiff_usercomment     RK123
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5999(8)
 0.4001(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. Uiso/Uaniso restraints and constraints
C79 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C178 \\sim C179
\\sim C177 \\sim C174 \\sim C176 \\sim C175: within 1A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C68 \\sim C73 \\sim C72 \\sim C71 \\sim C70 \\sim C69 \\sim C168 \\sim C173
\\sim C172 \\sim C171 \\sim C272 \\sim C273 \\sim C268 \\sim C269 \\sim C270
\\sim C271 \\sim C170 \\sim C169: within 1A with sigma of 0.01 and sigma for
terminal atoms of 0.01
4. Others
 1*[Sof(C272)+Sof(H272)+Sof(C273)+Sof(H273)+Sof(C268)+Sof(H268)+Sof(C269)+
 Sof(H269)+Sof(C270)+Sof(H270)+Sof(C271)+Sof(H271)]+1*[Sof(C68)+Sof(H68)+
 Sof(C73)+Sof(H73)+Sof(C72)+Sof(H72)+Sof(C71)+Sof(H71)+Sof(C70)+Sof(H70)+
 Sof(C69)+Sof(H69)]+1*[Sof(C168)+Sof(H168)+Sof(C173)+Sof(H173)+Sof(C172)+
 Sof(H172)+Sof(C171)+Sof(H171)+Sof(C170)+Sof(H170)+Sof(C169)+Sof(H169)]=1 with
 esd of 0
 Sof(C178)=Sof(H178)=Sof(C179)=Sof(H179)=Sof(C174)=Sof(H174)=Sof(C175)=
 Sof(H175)=Sof(C176)=Sof(H176)=Sof(C177)=Sof(H177)=1-FVAR(1)
 Sof(C79)=Sof(H79)=Sof(C74)=Sof(H74)=Sof(C75)=Sof(H75)=Sof(C76)=Sof(H76)=
 Sof(C77)=Sof(H77)=Sof(C78)=Sof(H78)=FVAR(1)
 Sof(C272)=Sof(H272)=Sof(C273)=Sof(H273)=Sof(C268)=Sof(H268)=Sof(C269)=
 Sof(H269)=Sof(C270)=Sof(H270)=Sof(C271)=Sof(H271)=FVAR(2)
 Sof(C68)=Sof(H68)=Sof(C73)=Sof(H73)=Sof(C72)=Sof(H72)=Sof(C71)=Sof(H71)=
 Sof(C70)=Sof(H70)=Sof(C69)=Sof(H69)=FVAR(3)
 Sof(C168)=Sof(H168)=Sof(C173)=Sof(H173)=Sof(C172)=Sof(H172)=Sof(C171)=
 Sof(H171)=Sof(C170)=Sof(H170)=Sof(C169)=Sof(H169)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C36(H36), C62(H62), C65(H65), C21(H21), C33(H33), C50(H50), C53(H53)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C17(H17), C19(H19), C29(H29), C31(H31), C41(H41), C18(H18),
 C59(H59), C60(H60), C48(H48), C58(H58), C68(H68), C73(H73), C72(H72), C71(H71),
  C70(H70), C69(H69), C79(H79), C74(H74), C75(H75), C76(H76), C77(H77),
 C78(H78), C30(H30), C47(H47), C46(H46), C168(H168), C173(H173), C172(H172),
 C171(H171), C170(H170), C169(H169), C178(H178), C179(H179), C174(H174),
 C175(H175), C176(H176), C177(H177), C272(H272), C273(H273), C268(H268),
 C269(H269), C270(H270), C271(H271)
5.c Fitted hexagon refined as free rotating group:
 C68(C73,C72,C71,C70,C69), C79(C74,C75,C76,C77,C78), C168(C173,C172,C171,C170,
 C169), C178(C179,C174,C175,C176,C177), C272(C273,C268,C269,C270,C271)
5.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C63(H63A,H63B,H63C), C14(H14A,H14B,
 H14C), C38(H38A,H38B,H38C), C66(H66A,H66B,H66C), C10(H10A,H10B,H10C), C34(H34A,
 H34B,H34C), C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C26(H26A,H26B,H26C),
 C55(H55A,H55B,H55C), C39(H39A,H39B,H39C), C64(H64A,H64B,H64C), C52(H52A,H52B,
 H52C), C22(H22A,H22B,H22C), C35(H35A,H35B,H35C), C67(H67A,H67B,H67C), C23(H23A,
 H23B,H23C), C54(H54A,H54B,H54C)
;
_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 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.774
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.9726\% 
 around [-0.00 0.00 1.00] (reciprocal) or [0.06 0.00 1.00] (direct)
;