Synthesis and Characterization of Rhodium Complexes with Phosphine-Stabilized Germylenes
Juan Manuel García; Edgar Ocando Mavárez; Tsuyoshi Kato; David Santiago Coll; Alexander Briceño; Nathalie Saffon-Merceron; Antoine Bacereido; Inorganic Chemistry 51 (2012) 8187–8193; doi:10.1021/ic300600c

data_4329822
_publ_contact_author_address
;
    Centro de Qu\'imica
    Instituto Venezolano de Investigaciones Cient\'ifica (IVIC)
    Apartado 21827
    Caracas 1020-A
    Venezuela
;
_publ_contact_author_email       abriceno@ivic.ve
_publ_contact_author_fax         '(58-212) 504-1350'
_publ_contact_author_name        'Dr. Alexander Brice\~no'
_publ_contact_author_phone       '(58-212) 504-1320'
_publ_section_title
;
 Synthesis and Characterization of Rhodium Complexes with
 Phosphine-Stabilized Germylenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8187
_journal_page_last               8193
_journal_paper_doi               10.1021/ic300600c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C41 H60 Cl Ge N3 P Rh, 0.5(C1 H2 Cl2) '
_chemical_formula_sum            'C41.5 H61 Cl2 Ge N3 P Rh'
_chemical_formula_weight         879.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 105.206(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.324(10)
_cell_length_b                   10.852(2)
_cell_length_c                   20.025(5)
_cell_measurement_reflns_used    2980
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.40
_cell_volume                     8456(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics
;
SHELXLTL-NT V5.1 (Bruker AXS, 1998) 
;
_computing_publication_material
; 
SHELXLTL-NT V5.1 (Bruker AXS, 1998).
;
_computing_structure_refinement  'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_computing_structure_solution    'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.780
_diffrn_measurement_device       'Mercury (2x2 bin mode)'
_diffrn_measurement_device_type  'Rigaku AFC7S Mercury'
_diffrn_measurement_method       '\w '
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47358
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
Attempts were made to model this disorder or split it 
into two positions, but were unsuccessful. 
PLATON/SQUEZZE routine was used to correct the data 
for the presence of a disordered solvent. A potential 
solvent volume of 582.7 \%A3 was found. 
The stoichiometry of the solvent was calculated to 
be approximately 0.5 molecules of Dichloromethane
per formula unit, which results in a total of 179
electrons per unit cell. This molecule was used to calculate 
expected molecular weight, DXcalc and F(000). 
;
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+57.4715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                6012
_reflns_number_total             7927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300600c_si_001_3.cif
_cod_data_source_block           2b1
_cod_original_cell_volume        8456(4)
_cod_original_formula_sum        'C41.50 H61 Cl2 Ge N3 P Rh'
_cod_database_code               4329822