Chalcogeno[bis(phosphaalkenyl)] Germanium and Tin Compounds
Tibor-Gabor Kocsor; Dimitri Matioszek; Gabriela Nemeş; Annie Castel; Jean Escudié; Petronela M. Petrar; Nathalie Saffon; Ionel Haiduc; Inorganic Chemistry 51 (2012) 7782–7787; doi:10.1021/ic300810q

data_4329722
_publ_section_title
;
 Chalcogeno[bis(phosphaalkenyl)] Germanium and Tin Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7782
_journal_page_last               7787
_journal_paper_doi               10.1021/ic300810q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C59.5 H90 Cl2 Ge N2 P2 Se'
_chemical_formula_weight         1117.73
_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                87.142(3)
_cell_angle_beta                 87.901(2)
_cell_angle_gamma                82.048(2)
_cell_formula_units_Z            4
_cell_length_a                   9.9799(5)
_cell_length_b                   22.0637(12)
_cell_length_c                   27.7366(15)
_cell_measurement_reflns_used    9202
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.65
_cell_measurement_theta_min      2.43
_cell_volume                     6038.4(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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker kappa APEX-II CCD Quazar'
_diffrn_measurement_method       'phi and omega 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  0.1033
_diffrn_reflns_av_sigmaI/netI    0.1230
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            100435
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_correction_T_min  0.6403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       needle
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1456
_refine_ls_number_reflns         20176
_refine_ls_number_restraints     783
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+13.2922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                12104
_reflns_number_total             20176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300810q_si_001_3.cif
_cod_data_source_block           5
_cod_original_formula_sum        'C59.50 H90 Cl2 Ge N2 P2 Se'
_cod_database_code               4329722