Synthesis of Heteroleptic Tin(II) and Lead(II) Compounds from Pyrazyl-Linked Bisphosphoranoimine
Leung, Wing-Por; Chan, Ka-Po; Kan, Kwok-Wai; Mak, Thomas C. W.; Organometallics 27 (2008) 2767–; doi:10.1021/om800104x

data_4071320
_publ_section_title
;
 Synthesis of Heteroleptic Tin(II) and Lead(II) Compounds from
 Pyrazyl-Linked Bisphosphoranoimine
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2767
_journal_paper_doi               10.1021/om800104x
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C34 H60 N4 P2 Si2 Sn2'
_chemical_formula_weight         880.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 102.609(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.645(7)
_cell_length_b                   16.011(6)
_cell_length_c                   15.407(6)
_cell_measurement_reflns_used    961
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.11
_cell_measurement_theta_min      2.69
_cell_volume                     4248(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28660
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.724086
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.993
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         10302
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+5.9631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                4626
_reflns_number_total             10302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800104x-file006.cif
_cod_data_source_block           ckp17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      P2(1)/c
_cod_database_code               4071320