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_4088938
_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         'C6 H11 O2 Re S3'
_chemical_formula_sum            'C6 H11 O2 Re S3'
_chemical_formula_weight         397.53
_chemical_name_common            LKR-606
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1938(3)
_cell_length_b                   11.5524(4)
_cell_length_c                   9.6348(3)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      36.3915
_cell_measurement_theta_min      2.7527
_cell_volume                     1023.32(6)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc.)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc.)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20288
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         2.75
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    12.445
_exptl_absorpt_correction_T_max  0.12
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.362
_exptl_crystal_size_min          0.290
_refine_diff_density_max         1.083
_refine_diff_density_min         -1.038
_refine_ls_extinction_coef       0.0054(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         2340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0170
_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^)+(0.0214P)^2^+0.7351P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0424
_reflns_number_gt                2250
_reflns_number_total             2340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00570_si_003.cif
_cod_data_source_block           I
_cod_database_code               4088938
_shelx_res_checksum              56806
_shelx_hkl_checksum              13434