Syntheses, Structures, and VT NMR Studies of Diselenophosphates of Group 14 Organometals. DFT Calculations for Gas-Phase Stability of Dinuclear Ions, [(Ph3M)2{μ-Se, Se-P(OR)2}]+(M = Ge, Sn, and Pb)
Liu, C. W.; Lobana, Tarlok S.; Xiao, Jie-Liang; Liu, Hong-Yuan; Liaw, Ben-Jie; Hung, Chiu-Ming; Lin, Zhenyang; Organometallics 24 (2005) 4072–; doi:10.1021/om050291q

data_4075915
_publ_section_title
;
 Syntheses, Structures, and VT NMR Studies of Diselenophosphates of Group
 14 Organometals. DFT Calculations for Gas-Phase Stability of Dinuclear
 Ions, [(Ph3M)2{\m-Se, Se-P(OR)2}]+(M = Ge, Sn, and Pb)
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4072
_journal_paper_doi               10.1021/om050291q
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C24 H29 O2 P Se2 Sn'
_chemical_formula_weight         657.05
_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                96.147(9)
_cell_angle_beta                 90.109(12)
_cell_angle_gamma                99.216(12)
_cell_formula_units_Z            2
_cell_length_a                   9.5653(15)
_cell_length_b                   10.4242(15)
_cell_length_c                   13.5634(16)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.43
_cell_measurement_theta_min      2.36
_cell_volume                     1327.0(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4193
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.99
_diffrn_standards_interval_count 297
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.783
_exptl_absorpt_correction_T_max  0.9977
_exptl_absorpt_correction_T_min  0.4912
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+3.7223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                3082
_reflns_number_total             3446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050291qsi20050416_053129.cif
_cod_data_source_block           6
_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_sg_symbol_H-M      P-1
_cod_database_code               4075915