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_4328746
_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
'C65 H59 Ge Ir O3 P4 Rh, C F3 O3 S, 1.5(C H2 Cl2), 0.5(C4 H10 O)'
_chemical_formula_sum            'C69.5 H67 Cl3 F3 Ge Ir O6.5 P4 Rh S'
_chemical_formula_weight         1693.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.4450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0440(9)
_cell_length_b                   24.1520(12)
_cell_length_c                   17.5193(9)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      2.30
_cell_volume                     7133.6(6)
_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    'SIR-97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            63884
_diffrn_reflns_theta_full        27.83
_diffrn_reflns_theta_max         27.83
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_T_max  0.7392
_exptl_absorpt_correction_T_min  0.5007
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.753
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         16865
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+15.1816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                13522
_reflns_number_total             16865
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2021269_si_003_9.cif
_cod_data_source_block           16
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C69.50 H67 Cl3 F3 Ge Ir O6.50 P4 Rh S'
_cod_database_code               4328746