Germyl- and Germylene-Bridged Complexes of Rh/Ir and Subsequent Chemistry of a Bridging Germylene Group
Md Hosnay Mobarok; Robert McDonald; Michael J. Ferguson; Martin Cowie; Inorganic Chemistry 51 (2012) 4020–4034; doi:10.1021/ic2021269

data_4328742
_publ_contact_author_address
; Department of Chemistry
  University of Alberta
  Edmonton, Alberta T6G 2G2
  Canada
;
_publ_contact_author_email       martin.cowie@ualberta.ca
_publ_contact_author_fax         1(780)4928231
_publ_contact_author_name        'Martin Cowie'
_publ_contact_author_phone       1(780)4925581
_publ_section_title
;
 Germyl- and Germylene-Bridged Complexes of Rh/Ir and Subsequent Chemistry
 of a Bridging Germylene Group
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4020
_journal_page_last               4034
_journal_paper_doi               10.1021/ic2021269
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C77 H66 Ge2 Ir O3 P4 Rh, 1.5(C6 H5 F)'
_chemical_formula_sum            'C86 H73.5 F1.5 Ge2 Ir O3 P4 Rh'
_chemical_formula_weight         1747.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.4832(4)
_cell_angle_beta                 104.7670(4)
_cell_angle_gamma                113.7850(4)
_cell_formula_units_Z            2
_cell_length_a                   13.4862(5)
_cell_length_b                   15.7589(6)
_cell_length_c                   20.9542(8)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.21
_cell_volume                     3801.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0095
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34726
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    2.878
_exptl_absorpt_correction_T_max  0.4429
_exptl_absorpt_correction_T_min  0.2348
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       prism
_exptl_crystal_F_000             1746
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.317
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         17540
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+2.5341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                16703
_reflns_number_total             17540
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2021269_si_003_5.cif
_cod_data_source_block           10
_cod_database_code               4328742