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_4316525
_publ_section_title
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 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 Pb2, C6 H14'
_chemical_formula_sum            'C66 H88 P2 Pb2'
_chemical_formula_weight         1357.70
_chemical_melting_point          274
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 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                 98.436(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.842(3)
_cell_length_b                   20.591(6)
_cell_length_c                   12.734(4)
_cell_measurement_reflns_used    8050
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.19
_cell_volume                     3071.4(15)
_computing_cell_refinement       'SAINT (7.60A) (Bruker, 2008)'
_computing_data_collection       'SMART (Version 5.054) (Bruker, 2002)'
_computing_data_reduction        'SAINT (7.60A) (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       '\w and \f'
_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  0.0743
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12523
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    5.563
_exptl_absorpt_correction_T_max  0.2611
_exptl_absorpt_correction_T_min  0.2144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_refine_diff_density_max         2.567
_refine_diff_density_min         -2.206
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3594
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0972P)^2^+0.6110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1607
_reflns_number_gt                2569
_reflns_number_total             3594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101068a_si_001_3.cif
_cod_data_source_block           wam08fmi
_cod_original_cell_volume        3071.6(15)
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               4316525