Syntheses of Molybdenum Oxo Benzylidene Complexes.
Zhai, Feng; Bukhryakov, Konstantin V.; Schrock, Richard R.; Hoveyda, Amir H.; Tsay, Charlene; Müller, Peter; Journal of the American Chemical Society 140 (2018) 13609–13613; doi:10.1021/jacs.8b09616

data_4133324
_publ_section_title
;
 Syntheses of Molybdenum Oxo Benzylidene Complexes.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13609
_journal_page_last               13613
_journal_paper_doi               10.1021/jacs.8b09616
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C56 H58 Mo O4'
_chemical_formula_weight         890.96
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/2
_cell_angle_alpha                90
_cell_angle_beta                 104.2469(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.9462(16)
_cell_length_b                   11.8211(6)
_cell_length_c                   27.6304(14)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.76
_cell_measurement_theta_min      2.49
_cell_volume                     10113.4(9)
_computing_cell_refinement       'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2017.3.0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/2 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            500433
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.577
_diffrn_reflns_theta_min         1.315
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.301
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.7156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         18399
_refine_ls_number_restraints     487
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+15.9228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16304
_reflns_number_total             18399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09616_si_005.cif
_cod_data_source_block           X18064_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4133324
_shelx_shelxl_version_number     2017/2
_shelx_estimated_absorpt_t_min   0.931
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              65006
_shelx_hkl_checksum              30968
_shelx_fab_checksum              42855