Metal-Only Lewis Pairs Based on Zerovalent Osmium
Bissert, Robin; Braunschweig, Holger; Dewhurst, Rian D.; Schneider, Christoph; Organometallics 35 (2016) 2567–; doi:10.1021/acs.organomet.6b00495

data_4088854
_publ_section_title
;
 Metal-Only Lewis Pairs Based on Zerovalent Osmium
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              2567
_journal_paper_doi               10.1021/acs.organomet.6b00495
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C7 H9 Cl3 Ga O4 Os P'
_chemical_formula_sum            'C7 H9 Cl3 Ga O4 Os P'
_chemical_formula_weight         554.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   iterative
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5020(5)
_cell_length_b                   8.8053(3)
_cell_length_c                   13.5439(5)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.76
_cell_volume                     1490.96(10)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS area detector (Photon 100)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49864
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.758
_diffrn_reflns_theta_min         2.759
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_exptl_absorpt_coefficient_mu    10.962
_exptl_absorpt_correction_T_max  0.3975
_exptl_absorpt_correction_T_min  0.2641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/2 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.794
_refine_diff_density_min         -2.429
_refine_diff_density_rms         0.402
_refine_ls_abs_structure_details
;
 Flack x determined using 1343 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.454
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3044
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.454
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.1523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.917
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                3000
_reflns_number_total             3044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00495_si_002.cif
_cod_data_source_block           2a
_cod_database_code               4088854
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.240
_shelx_estimated_absorpt_t_max   0.456
_shelx_res_checksum              65233