Synthesis of Heavier Group 14 Metal Compounds from 2,6-Lutidylbis(phosphoranosulfide)
Leung, Wing-Por; Kan, Kwok-Wai; Mak, Thomas C. W.; Organometallics 29 (2010) 1890–; doi:10.1021/om1001167

data_4065760
_publ_section_title
;
 Synthesis of Heavier Group 14 Metal Compounds from
 2,6-Lutidylbis(phosphoranosulfide)
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1890
_journal_paper_doi               10.1021/om1001167
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C38 H68 Cl4 Ge3 N2 P4 S4'
_chemical_formula_weight         1164.63
_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                95.876(3)
_cell_angle_beta                 92.024(3)
_cell_angle_gamma                93.584(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0484(12)
_cell_length_b                   13.2864(18)
_cell_length_c                   22.754(3)
_cell_measurement_reflns_used    936
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.49
_cell_volume                     2713.4(6)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            18630
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    2.148
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.162325
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         12890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0578P)^2^+0.0395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                8231
_reflns_number_total             12890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1001167_si_001.cif
_cod_data_source_block           kkw65
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2713.5(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065760