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_4125313
_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            'C42.5 H55 Cl N2 O W'
_chemical_formula_weight         829.18
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 103.3269(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.575(4)
_cell_length_b                   8.4965(7)
_cell_length_c                   23.441(2)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.19
_cell_measurement_theta_min      2.40
_cell_volume                     7863.6(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7195
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.352
_diffrn_reflns_theta_min         1.031
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    3.039
_exptl_absorpt_correction_T_max  0.6478
_exptl_absorpt_correction_T_min  0.5346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.719
_refine_diff_density_min         -1.549
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7195
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0073P)^2^+34.5112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6658
_reflns_number_total             7195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10499_si_003.cif
_cod_data_source_block           X16163
_cod_depositor_comments
'Adding full bibliography for 4125313--4125315.cif.'
_cod_original_cell_volume        7863.7(12)
_cod_original_formula_sum        'C42.50 H55 Cl N2 O W'
_cod_database_code               4125313
_shelx_estimated_absorpt_t_min   0.749
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2014/6
_shelx_res_checksum              19618
_shelx_hkl_checksum              22252