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_4088942
_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         'C7 H13 O2 Re S3'
_chemical_formula_sum            'C7 H13 O2 Re S3'
_chemical_formula_weight         411.55
_chemical_name_common            LKR-847
_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
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.2600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.6520(4)
_cell_length_b                   14.5211(6)
_cell_length_c                   14.9039(6)
_cell_measurement_reflns_used    616
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      33.8392
_cell_measurement_theta_min      2.7955
_cell_volume                     2298.95(16)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59081
_diffrn_reflns_theta_full        35.17
_diffrn_reflns_theta_max         35.17
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    11.083
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.241
_refine_diff_density_max         1.387
_refine_diff_density_min         -0.922
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         10204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0202
_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^)+(0.0144P)^2^+1.8390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0406
_reflns_number_gt                9209
_reflns_number_total             10204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00570_si_003.cif
_cod_data_source_block           rds293
_cod_database_code               4088942
_shelx_res_checksum              7582
_shelx_hkl_checksum              73768