Syntheses of Molybdenum Oxo Alkylidene Complexes through Addition of Water to an Alkylidyne Complex.
Bukhryakov, Konstantin V.; Schrock, Richard R.; Hoveyda, Amir H.; Tsay, Charlene; Müller, Peter; Journal of the American Chemical Society 140 (2018) 2797–2800; doi:10.1021/jacs.8b00499

data_4132032
_publ_section_title
;
 Syntheses of Molybdenum Oxo Alkylidene Complexes through Addition of
 Water to an Alkylidyne Complex.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2797
_journal_page_last               2800
_journal_paper_doi               10.1021/jacs.8b00499
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C52 H78 Cl Mo O3 P'
_chemical_formula_weight         913.50
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.302(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.0030(11)
_cell_length_b                   24.0118(13)
_cell_length_c                   23.9393(15)
_cell_measurement_reflns_used    9578
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.76
_cell_measurement_theta_min      2.21
_cell_volume                     10348.4(11)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Photon2 CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            412289
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.032
_diffrn_reflns_theta_min         2.039
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.7349
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_refine_diff_density_max         2.186
_refine_diff_density_min         -2.721
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1176
_refine_ls_number_reflns         35966
_refine_ls_number_restraints     416
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1345P)^2^+13.3849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30651
_reflns_number_total             35966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00499_si_002.cif
_cod_data_source_block           P17048
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132032
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              3917
_shelx_hkl_checksum              52143