Molybdenum and Tungsten Alkylidene and Metallacyclobutane Complexes That Contain a Dianionic Biphenolate Pincer Ligand
Sues, Peter E.; John, Jeremy M.; Schrock, Richard R.; Müller, Peter; Organometallics 35 (2016) 758–; doi:10.1021/acs.organomet.5b00976

data_4086419
_publ_section_title
;
 Molybdenum and Tungsten Alkylidene and Metallacyclobutane Complexes That
 Contain a Dianionic Biphenolate Pincer Ligand
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              758
_journal_paper_doi               10.1021/acs.organomet.5b00976
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C51.5 H61 F5 Mo N2 O2'
_chemical_formula_weight         930.96
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 114.468(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.326(11)
_cell_length_b                   16.556(6)
_cell_length_c                   17.670(6)
_cell_measurement_reflns_used    9191
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.21
_cell_volume                     9140(5)
_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 0.999
_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_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            148096
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_min         1.304
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3896
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.179
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         12817
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0514P)^2^+13.1421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10023
_reflns_number_total             12817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00976_si_002.cif
_cod_data_source_block           x15136
_cod_depositor_comments
'Adding full bibliography for 4086418--4086419.cif.'
_cod_original_formula_sum        'C51.50 H61 F5 Mo N2 O2'
_cod_database_code               4086419
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2014/6
_shelx_res_checksum              83484
_shelx_hkl_checksum              9787