CO Coupling Chemistry of a Terminal Mo Carbide: Sequential Addition of Proton, Hydride, and CO Releases Ethenone.
Buss, Joshua A.; Bailey, Gwendolyn A.; Oppenheim, Julius; VanderVelde, David G.; Goddard, 3rd, William A; Agapie, Theodor; Journal of the American Chemical Society 141 (2019) 15664–15674; doi:10.1021/jacs.9b07743

data_4127993
_publ_section_title
;
 CO Coupling Chemistry of a Terminal Mo Carbide: Sequential Addition of
 Proton, Hydride, and CO Releases Ethenone.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15664
_journal_page_last               15674
_journal_paper_doi               10.1021/jacs.9b07743
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C32 H42 Mo O P2, 0.5(C7 H8)'
_chemical_formula_sum            'C35.5 H42 Mo O P2'
_chemical_formula_weight         642.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-22
_audit_creation_method
;
Olex2 1.2
(compiled Apr  3 2018 11:26:26 for OlexSys, GUI svn.r5486)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.50(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.82(2)
_cell_length_b                   21.933(9)
_cell_length_c                   13.402(5)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.28
_cell_measurement_theta_min      2.88
_cell_volume                     6266(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46685
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         81.142
_diffrn_reflns_theta_min         2.891
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.581
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1074 before and 0.0575 after correction. The Ratio of minimum to maximum transmission is 0.8275. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0561P)^2^+18.8423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6253
_reflns_number_total             6683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07743_si_002.cif
_cod_data_source_block           6
_cod_original_cell_volume        6266(7)
_cod_original_formula_sum        'C35.50 H42 Mo O P2'
_cod_database_code               4127993
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.481
_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. Others
 Fixed Sof: C35(0.5) H35(0.5) C37(0.5) H37(0.5) C33(0.5) H33A(0.5) H33B(0.5)
 H33C(0.5) C36(0.5) H36(0.5) C38(0.5) H38(0.5) C34(0.5) C39(0.5) H39(0.5)
3.a Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C14(H14), C17(H17), C1(H1), C28(H28), C25(H25), C4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
3.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C10(H10), C9(H9), C8(H8), C20(H20), C11(H11), C22(H22), C23(H23),
 C35(H35), C37(H37), C36(H36), C38(H38), C39(H39)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C27(H27A,
 H27B,H27C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C),
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              75016
_shelx_hkl_checksum              95843
_olex2_submission_special_instructions 'No special instructions were received'