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_4329720
_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            'C49 H78 Cl2 N2 P2 Sn'
_chemical_formula_weight         946.66
_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                66.4910(10)
_cell_angle_beta                 69.4920(10)
_cell_angle_gamma                73.1300(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8737(2)
_cell_length_b                   15.0045(3)
_cell_length_c                   16.0067(3)
_cell_measurement_reflns_used    8380
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      4.08
_cell_volume                     2614.52(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35801
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.9348
_exptl_absorpt_correction_T_min  0.8754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXs)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         12828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0472P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                10135
_reflns_number_total             12828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300810q_si_001_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        2614.52(8)
_cod_database_code               4329720