Molybdenum and Tungsten Alkylidene Complexes That Contain a 2-Pyridyl-Substituted Phenoxide Ligand
Sues, Peter E.; John, Jeremy M.; Bukhryakov, Konstantin V.; Schrock, Richard R.; Müller, Peter; Organometallics 35 (2016) 3587–; doi:10.1021/acs.organomet.6b00644

data_4089023
_publ_section_title
;
 Molybdenum and Tungsten Alkylidene Complexes That Contain a
 2-Pyridyl-Substituted Phenoxide Ligand
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3587
_journal_paper_doi               10.1021/acs.organomet.6b00644
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C44 H40 Cl F5 Mo N2 O'
_chemical_formula_weight         839.17
_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'
_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                 104.780(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4635(18)
_cell_length_b                   16.5228(14)
_cell_length_c                   23.384(2)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      2.36
_cell_volume                     7644.9(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.0913
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21221
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_min         1.526
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.746070
_exptl_absorpt_correction_T_min  0.542269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.235
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         21221
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+12.3120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16403
_reflns_number_total             21221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00644_si_001.cif
_cod_data_source_block           X16005_t4
_cod_original_cell_volume        7644.8(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089023
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.897
_shelxl_version_number           2014/6
_shelx_res_checksum              81096
_shelx_hkl_checksum              12632