Reductive Carbonylation of Oxorhenium Hydrides Induced by Lewis Acids
Lambic, Nikola S.; Lilly, Cassandra P.; Robbins, Leanna K.; Sommer, Roger D.; Ison, Elon A.; Organometallics 35 (2016) 2822–; doi:10.1021/acs.organomet.6b00393

data_4088762
_publ_section_title
;
 Reductive Carbonylation of Oxorhenium Hydrides Induced by Lewis Acids
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2822
_journal_paper_doi               10.1021/acs.organomet.6b00393
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C17 H12 F10 N3 O Re'
_chemical_formula_sum            'C17 H12 F10 N3 O Re'
_chemical_formula_weight         650.50
_chemical_name_common            1175
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.836(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1014(4)
_cell_length_b                   19.6607(9)
_cell_length_c                   11.7352(6)
_cell_measurement_reflns_used    8458
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      33.7628
_cell_measurement_theta_min      2.9429
_cell_volume                     1862.52(16)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS Inc., 2009)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS Inc., 2009)'
_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 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  0.0699
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36374
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.638
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.125
_refine_diff_density_max         4.625
_refine_diff_density_min         -4.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         7270
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+9.1645P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                5410
_reflns_number_total             7270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00393_si_002.cif
_cod_data_source_block           rds117
_cod_database_code               4088762
_shelx_res_checksum              50292
_shelx_hkl_checksum              68469