Effect of the Ancillary Ligand on the Mechanism for CO Migratory Insertion in High-Valent Oxorhenium Complexes
Robbins, Leanna K.; Lilly, Cassandra P.; Sommer, Roger D.; Ison, Elon A.; Organometallics 35 (2016) 3530–; doi:10.1021/acs.organomet.6b00570

data_4088943
_publ_section_title
;
 Effect of the Ancillary Ligand on the Mechanism for CO Migratory
 Insertion in High-Valent Oxorhenium Complexes
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3530
_journal_paper_doi               10.1021/acs.organomet.6b00570
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C12 H16 O4 Re2 S6'
_chemical_formula_sum            'C12 H16 O4 Re2 S6'
_chemical_formula_weight         789.01
_chemical_name_common            'LKR 879'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 106.025(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6120(5)
_cell_length_b                   8.9891(4)
_cell_length_c                   19.1466(9)
_cell_measurement_reflns_used    321
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      31.2315
_cell_measurement_theta_min      2.5201
_cell_volume                     1920.89(15)
_computing_cell_refinement       'APEX2 v2014.5-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            68912
_diffrn_reflns_theta_full        36.41
_diffrn_reflns_theta_max         36.41
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    13.258
_exptl_absorpt_correction_T_max  0.61
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.556
_refine_diff_density_min         -1.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         9359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0205P)^2^+0.9555P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0472
_reflns_number_gt                7930
_reflns_number_total             9359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00570_si_003.cif
_cod_data_source_block           I
_cod_database_code               4088943
_shelx_res_checksum              2771
_shelx_hkl_checksum              76357