Synthesis and Characterization of the M(II) (M = Ge, Sn, or Pb) Phosphinidene Dimers {M(μ-PAr')}2 (Ar' = C6H3-2,6-(C6H3-2,6-Pri2)2)
W. Alexander Merrill; Eric Rivard; Jeffrey S. DeRopp; Xinping Wang; Bobby D. Ellis; James C. Fettinger; Bernd Wrackmeyer; Philip P. Power; Inorganic Chemistry 49 (2010) 8481–8486; doi:10.1021/ic101068a

data_4316524
_publ_section_title
;
 Synthesis and Characterization of the M(II) (M = Ge, Sn, or Pb)
 Phosphinidene Dimers {M(\m-PAr')}2 (Ar' = C6H3-2,6-(C6H3-2,6-Pri2)2)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8481
_journal_page_last               8486
_journal_paper_doi               10.1021/ic101068a
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C60 H74 P2 Sn2, C6 H14'
_chemical_formula_sum            'C66 H88 P2 Sn2'
_chemical_formula_weight         1180.68
_chemical_melting_point          332
_chemical_name_common            '[Dipp*PSn]2.hexane'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 128.261(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.0315(16)
_cell_length_b                   20.514(2)
_cell_length_c                   11.8910(12)
_cell_measurement_reflns_used    6125
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      2.5
_cell_volume                     3070.6(5)
_computing_cell_refinement       'SAINT 6.45A (Bruker, 2003)'
_computing_data_collection       'SMART 5.054 (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21241
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.8401
_exptl_absorpt_correction_T_min  0.7142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.780
_refine_diff_density_min         -3.946
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         4084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0000P)^2^+23.8048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                3041
_reflns_number_total             4084
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101068a_si_001_2.cif
_cod_data_source_block           rw4
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4316524