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_4086418
_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            'C49.5 H67 F5 Mo N2 O2'
_chemical_formula_weight         912.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                86.8869(15)
_cell_angle_beta                 72.7558(14)
_cell_angle_gamma                73.8698(15)
_cell_formula_units_Z            2
_cell_length_a                   10.9212(7)
_cell_length_b                   14.2236(9)
_cell_length_c                   16.8940(11)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.46
_cell_measurement_theta_min      2.53
_cell_volume                     2406.5(3)
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            115547
_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         30.998
_diffrn_reflns_theta_min         1.263
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.897
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         15334
_refine_ls_number_restraints     695
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0388P)^2^+1.6460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13639
_reflns_number_total             15334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00976_si_003.cif
_cod_data_source_block           X15138
_cod_depositor_comments
'Adding full bibliography for 4086418--4086419.cif.'
_cod_original_formula_sum        'C49.50 H67 F5 Mo N2 O2'
_cod_database_code               4086418
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2014/6
_shelx_res_checksum              54065
_shelx_hkl_checksum              76214