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_4328744
_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_sum            'C104 H109 B Ge Ir O6 P4 Rh'
_chemical_formula_weight         1957.30
_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                96.1547(3)
_cell_angle_beta                 108.3519(3)
_cell_angle_gamma                97.5944(4)
_cell_formula_units_Z            2
_cell_length_a                   14.1513(4)
_cell_length_b                   16.7686(5)
_cell_length_c                   20.6792(6)
_cell_measurement_reflns_used    9354
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.24
_cell_volume                     4558.6(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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40961
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    2.087
_exptl_absorpt_correction_T_max  0.7968
_exptl_absorpt_correction_T_min  0.5406
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered or 
partial-occupancy solvent tetrahydrofuran oxygen or carbon atoms were 
unsuccessful for two of the solvent sites within the crystal lattice.  The 
data were corrected for disordered electron density through use of the 
SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, 
A46, 194-201) as implemented in PLATON (Spek, A. L. Acta Crystallogr. 1990, 
A46, C34; Spek, A. L. J. Appl. Cryst. 2003, 36, 7-13.  PLATON - a 
multipurpose crystallographic tool.  Utrecht University, Utrecht, The 
Netherlands).  A total solvent-accessible void volume of 674 cubic
Angstroms with a total electron count of 167 (consistent with 4
molecules of solvent tetrahydrofuran, or 2 molecules per formula unit
of the RhIr complex) was found in the unit cell.
;
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         20835
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0455P)^2^+0.7951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                18288
_reflns_number_total             20835
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2021269_si_003_7.cif
_cod_data_source_block           14
_cod_database_code               4328744