Synthesis of Hetero-Binuclear Complexes from Bisgermavinylidene
Wing-Por Leung; Kwok-Wai Kan; Yuk-Chi Chan; Thomas C. W. Mak; Inorganic Chemistry 52 (2013) 4571–4577; doi:10.1021/ic400056f

data_4334502
_publ_section_title
;
 Synthesis of Hetero-Binuclear Complexes from Bisgermavinylidene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4571
_journal_page_last               4577
_journal_paper_doi               10.1021/ic400056f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C33.25 H42.5 Cl2.5 Fe Ge N2 O0.5 P2 Si2'
_chemical_formula_weight         813.38
_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                 104.585(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.371(5)
_cell_length_b                   11.1108(13)
_cell_length_c                   19.497(2)
_cell_measurement_reflns_used    934
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.67
_cell_measurement_theta_min      2.25
_cell_volume                     8882.9(17)
_computing_cell_refinement       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_collection       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_reduction        'BRUKER SMART CCD DIFFRACTOMETER'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23438
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    1.303
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.500261
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         7809
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+23.3355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.2007
_reflns_number_gt                5394
_reflns_number_total             7809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400056f_si_006.cif
_cod_data_source_block           kkw70
_cod_original_cell_volume        8882.8(18)
_cod_original_formula_sum        'C33.25 H42.50 Cl2.50 Fe Ge N2 O0.50 P2 Si2'
_cod_database_code               4334502