Mechanism for the Reaction of CO with Oxorhenium Hydrides: Migratory Insertion of CO into Rhenium Hydride and Formyl Bonds leads to Migration from Rhenium to the Oxo Ligand
Lambic, Nikola S.; Lilly, Cassandra P.; Sommer, Roger D.; Ison, Elon A.; Organometallics 35 (2016) 3060–; doi:10.1021/acs.organomet.6b00591

data_4088974
_publ_section_title
;
 Mechanism for the Reaction of CO with Oxorhenium Hydrides: Migratory
 Insertion of CO into Rhenium Hydride and Formyl Bonds leads to Migration
 from Rhenium to the Oxo Ligand
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3060
_journal_paper_doi               10.1021/acs.organomet.6b00591
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C38 H24 F20 N6 O6 Re2, C7 H8'
_chemical_formula_sum            'C45 H32 F20 N6 O6 Re2'
_chemical_formula_weight         1505.16
_chemical_name_common            formate
_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   mixed
_cell_angle_alpha                90
_cell_angle_beta                 97.0360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7430(2)
_cell_length_b                   24.9855(7)
_cell_length_c                   23.0492(7)
_cell_measurement_reflns_used    2500
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.7157
_cell_measurement_theta_min      2.3304
_cell_volume                     4997.1(2)
_computing_cell_refinement       'APEX3 v2015.5-2 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100.(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  0.0433
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            95196
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.86
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.969
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.726
_refine_diff_density_min         -2.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.267
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         12419
_refine_ls_number_restraints     877
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0162P)^2^+30.1949P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                10750
_reflns_number_total             12419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00591_si_003.cif
_cod_data_source_block           rds316
_cod_database_code               4088974
_shelx_res_checksum              39128
_shelx_hkl_checksum              4749