Synthesis and characterization of Sn(II), Pb(II) and Yb(II) complexes supported by [C(Ph2PNSiMe3){6-(2-RC5H3N)}]2− or [CH(Ph2PNSiMe3){6-(2-RC5H3N)}]− (R = 3,5-dimethyl-1-pyrazolyl or iminophosphoranyl) ligands
Chai, Zuo-Yun; Wang, Zhong-Xia; Dalton Transactions  (2009) 8005–8012; doi:10.1039/b906266a

data_7002304
_publ_section_title
;
 Synthesis and characterization of Sn(II), Pb(II) and Yb(II) complexes
 supported by [C(Ph2P&#xE001;NSiMe3){6-(2-RC5H3N)}]2&#x2212; or
 [CH(Ph2P&#xE001;NSiMe3){6-(2-RC5H3N)}]&#x2212; (R =
 3,5-dimethyl-1-pyrazolyl or iminophosphoranyl) ligands
;
_journal_issue                   38
_journal_name_full               'Dalton Transactions'
_journal_page_first              8005
_journal_page_last               8012
_journal_paper_doi               10.1039/b906266a
_journal_year                    2009
_chemical_formula_sum            'C76 H90 N6 O P4 Pb2 Si4'
_chemical_formula_weight         1754.16
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.789(2)
_cell_length_b                   17.829(2)
_cell_length_c                   22.813(3)
_cell_measurement_reflns_used    4597
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.843
_cell_measurement_theta_min      2.643
_cell_volume                     8455.6(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1288
_diffrn_reflns_av_sigmaI/netI    0.1232
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40850
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    4.152
_exptl_absorpt_correction_T_max  0.5563
_exptl_absorpt_correction_T_min  0.4485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.476
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7463
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1473
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                3417
_reflns_number_total             7463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906266a.txt
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        8455.3(17)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7002304