Synthesis and Evaluation of Molybdenum and Tungsten Monoaryloxide Halide Alkylidene Complexes for Z-Selective Cross-Metathesis of Cyclooctene and Z-1,2-Dichloroethylene.
Lam, Jonathan K.; Zhu, Congqing; Bukhryakov, Konstantin V.; Müller, Peter; Hoveyda, Amir; Schrock, Richard R.; Journal of the American Chemical Society 138 (2016) 15774–15783; doi:10.1021/jacs.6b10499

data_4125315
_publ_section_title
;
 Synthesis and Evaluation of Molybdenum and Tungsten Monoaryloxide Halide
 Alkylidene Complexes for Z-Selective Cross-Metathesis of Cyclooctene and
 Z-1,2-Dichloroethylene.
;
_journal_issue                   48
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15774
_journal_page_last               15783
_journal_paper_doi               10.1021/jacs.6b10499
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C51 H63 Cl Mo N2 O'
_chemical_formula_weight         851.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 110.024(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.729(5)
_cell_length_b                   11.107(2)
_cell_length_c                   21.689(5)
_cell_measurement_reflns_used    9458
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.68
_cell_measurement_theta_min      2.18
_cell_volume                     4691.7(18)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-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 0.998
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            143485
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.676
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.7043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.515
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.225
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         14282
_refine_ls_number_restraints     418
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0295P)^2^+2.4178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12598
_reflns_number_total             14282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10499_si_002.cif
_cod_data_source_block           X16049
_cod_depositor_comments
'Adding full bibliography for 4125313--4125315.cif.'
_cod_original_cell_volume        4691.6(18)
_cod_database_code               4125315
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.921
_shelxl_version_number           2014/6
_shelx_res_checksum              78809
_shelx_hkl_checksum              8252