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_4127994
_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         'C35 H50 Mo O P2 Si, C2 H5'
_chemical_formula_sum            'C37 H55 Mo O P2 Si'
_chemical_formula_weight         701.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155),
SHELXL-2014,
and manual edit
;
_cell_angle_alpha                94.987(2)
_cell_angle_beta                 105.434(2)
_cell_angle_gamma                110.315(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6736(5)
_cell_length_b                   12.0522(5)
_cell_length_c                   14.3227(6)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.94
_cell_measurement_theta_min      2.44
_cell_volume                     1785.40(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT-2014/4 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD Area Detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            174061
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         37.941
_diffrn_reflns_theta_min         1.838
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.7475
_exptl_absorpt_correction_T_min  0.7008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0551 before and 0.0506 after correction. The Ratio of minimum to maximum transmission is 0.9375. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         18619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.4021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15458
_reflns_number_total             18619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07743_si_002.cif
_cod_data_source_block           11
_cod_original_cell_volume        1785.40(13)
_cod_database_code               4127994
_shelxl_version_number           2014-7
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.890
_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.a Ternary CH refined with riding coordinates:
 C22(H22), C28(H28), C19(H19), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C9(H9), C18(H18), C3(H3), C32(H32), C2(H2), C15(H15),
 C17(H17), C12(H12), C16(H16), C11(H11), C10(H10)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C30(H30A,H30B,
 H30C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C20(H20A,
 H20B,H20C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'