#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:25:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179245 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/65/4316524.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4316524
loop_
_publ_author_name
'W. Alexander Merrill'
'Eric Rivard'
'Jeffrey S. DeRopp'
'Xinping Wang'
'Bobby D. Ellis'
'James C. Fettinger'
'Bernd Wrackmeyer'
'Philip P. Power'
_publ_section_title
;
 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)
;
_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       ω
_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/[σ²(Fo²)+(0.0000P)²+23.8048P] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.62529(3) 0.5000 0.67511(5) 0.04292(17) Uani 1 2 d S . .
P1 P 0.53153(13) 0.57534(8) 0.47662(19) 0.0185(4) Uani 0.50 1 d P . .
C1 C 0.5000 0.6616(3) 0.5000 0.0460(19) Uani 1 2 d S . .
C2 C 0.5860(3) 0.69651(18) 0.6192(4) 0.0287(9) Uani 1 1 d . . .
C3 C 0.5842(3) 0.76415(17) 0.6166(4) 0.0278(8) Uani 1 1 d . . .
H3A H 0.6421 0.7876 0.6965 0.033 Uiso 1 1 calc R . .
C4 C 0.5000 0.7982(2) 0.5000 0.0321(13) Uani 1 2 d S . .
H4A H 0.5000 0.8445 0.5000 0.039 Uiso 1 2 calc SR . .
C5 C 0.6788(3) 0.66187(17) 0.7485(4) 0.0237(8) Uani 1 1 d . . .
C6 C 0.7667(3) 0.64469(18) 0.7555(4) 0.0267(8) Uani 1 1 d . . .
C7 C 0.8519(3) 0.6124(2) 0.8764(4) 0.0316(9) Uani 1 1 d . . .
H7A H 0.9117 0.6008 0.8820 0.038 Uiso 1 1 calc R . .
C8 C 0.8504(3) 0.5970(2) 0.9888(4) 0.0320(9) Uani 1 1 d . . .
H8A H 0.9087 0.5747 1.0704 0.038 Uiso 1 1 calc R . .
C9 C 0.7638(3) 0.6144(2) 0.9816(4) 0.0310(9) Uani 1 1 d . . .
H9A H 0.7633 0.6038 1.0590 0.037 Uiso 1 1 calc R . .
C10 C 0.6771(3) 0.64722(19) 0.8628(4) 0.0264(8) Uani 1 1 d . . .
C11 C 0.7733(4) 0.6619(2) 0.6372(5) 0.0356(10) Uani 1 1 d . . .
H11A H 0.7013 0.6766 0.5524 0.043 Uiso 1 1 calc R . .
C12 C 0.8061(5) 0.6047(3) 0.5897(6) 0.0553(15) Uani 1 1 d . . .
H12A H 0.7580 0.5679 0.5624 0.083 Uiso 1 1 calc R . .
H12B H 0.8790 0.5917 0.6688 0.083 Uiso 1 1 calc R . .
H12C H 0.8023 0.6180 0.5075 0.083 Uiso 1 1 calc R . .
C13 C 0.8505(4) 0.7187(2) 0.6840(5) 0.0479(13) Uani 1 1 d . . .
H13A H 0.8253 0.7569 0.7048 0.072 Uiso 1 1 calc R . .
H13B H 0.8543 0.7293 0.6069 0.072 Uiso 1 1 calc R . .
H13C H 0.9212 0.7064 0.7701 0.072 Uiso 1 1 calc R . .
C14 C 0.5848(3) 0.6669(2) 0.8615(4) 0.0356(10) Uani 1 1 d . . .
H14A H 0.5349 0.6934 0.7732 0.043 Uiso 1 1 calc R . .
C15 C 0.6213(4) 0.7091(2) 0.9874(6) 0.0478(13) Uani 1 1 d . . .
H15A H 0.6628 0.7456 0.9924 0.072 Uiso 1 1 calc R . .
H15B H 0.6655 0.6833 1.0755 0.072 Uiso 1 1 calc R . .
H15C H 0.5593 0.7258 0.9763 0.072 Uiso 1 1 calc R . .
C16 C 0.5244(5) 0.6100(3) 0.8539(11) 0.127(4) Uani 1 1 d . . .
H16A H 0.4678 0.6251 0.8568 0.190 Uiso 1 1 calc R . .
H16B H 0.5724 0.5811 0.9354 0.190 Uiso 1 1 calc R . .
H16C H 0.4931 0.5862 0.7644 0.190 Uiso 1 1 calc R . .
C17 C 0.9436(7) 0.5000 0.4700(12) 0.073(3) Uani 1 2 d S . .
H17 H 0.9317 0.4623 0.5062 0.088 Uiso 1 1 d R . .
C18 C 0.8625(9) 0.5000 0.3144(12) 0.109(4) Uani 1 2 d S . .
H18 H 0.8740 0.4623 0.2778 0.131 Uiso 1 1 d R . .
C19 C 0.7472(8) 0.5000 0.2528(12) 0.081(3) Uani 1 2 d S . .
H19A H 0.7011 0.5000 0.1500 0.122 Uiso 1 2 d SR . .
H19B H 0.7338 0.4618 0.2861 0.122 Uiso 1 1 d R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Sn1 P1 79.64(8) 6_565 . ?
P1 Sn1 P1 33.47(9) 6_565 5_666 ?
P1 Sn1 P1 87.22(6) . 5_666 ?
P1 Sn1 P1 87.22(6) 6_565 2_656 ?
P1 Sn1 P1 33.47(9) . 2_656 ?
P1 Sn1 P1 75.68(8) 5_666 2_656 ?
P1 P1 C1 68.10(8) 2_656 . ?
P1 P1 Sn1 77.35(11) 2_656 . ?
C1 P1 Sn1 120.82(10) . . ?
P1 P1 Sn1 69.19(10) 2_656 5_666 ?
C1 P1 Sn1 115.89(9) . 5_666 ?
Sn1 P1 Sn1 92.78(6) . 5_666 ?
C2 C1 C2 119.3(5) . 2_656 ?
C2 C1 P1 120.3(2) . 2_656 ?
C2 C1 P1 115.7(2) 2_656 2_656 ?
C2 C1 P1 115.7(2) . . ?
C2 C1 P1 120.3(2) 2_656 . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 C5 119.4(3) . . ?
C1 C2 C5 121.3(3) . . ?
C4 C3 C2 121.4(4) . . ?
C4 C3 H3A 119.3 . . ?
C2 C3 H3A 119.3 . . ?
C3 C4 C3 119.4(5) 2_656 . ?
C3 C4 H4A 120.3 2_656 . ?
C3 C4 H4A 120.3 . . ?
C6 C5 C10 120.5(3) . . ?
C6 C5 C2 120.1(4) . . ?
C10 C5 C2 119.4(4) . . ?
C7 C6 C5 119.2(4) . . ?
C7 C6 C11 118.8(4) . . ?
C5 C6 C11 122.1(4) . . ?
C8 C7 C6 120.8(4) . . ?
C8 C7 H7A 119.6 . . ?
C6 C7 H7A 119.6 . . ?
C9 C8 C7 119.8(4) . . ?
C9 C8 H8A 120.1 . . ?
C7 C8 H8A 120.1 . . ?
C8 C9 C10 121.2(4) . . ?
C8 C9 H9A 119.4 . . ?
C10 C9 H9A 119.4 . . ?
C9 C10 C5 118.5(4) . . ?
C9 C10 C14 119.3(4) . . ?
C5 C10 C14 122.1(3) . . ?
C6 C11 C12 113.7(4) . . ?
C6 C11 C13 110.2(3) . . ?
C12 C11 C13 109.5(4) . . ?
C6 C11 H11A 107.8 . . ?
C12 C11 H11A 107.8 . . ?
C13 C11 H11A 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C16 C14 C15 110.5(5) . . ?
C16 C14 C10 112.7(4) . . ?
C15 C14 C10 111.5(4) . . ?
C16 C14 H14A 107.3 . . ?
C15 C14 H14A 107.3 . . ?
C10 C14 H14A 107.3 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C17 118.4(12) . 5_766 ?
C18 C17 H17 107.4 . . ?
C17 C17 H17 107.9 5_766 . ?
C17 C18 C19 118.5(10) . . ?
C17 C18 H18 107.7 . . ?
C19 C18 H18 107.5 . . ?
C18 C19 H19A 111.3 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 P1 2.4134(18) 6_565 ?
Sn1 P1 2.4134(18) . ?
Sn1 P1 2.5192(17) 5_666 ?
Sn1 P1 2.5192(17) 2_656 ?
P1 P1 1.424(4) 2_656 ?
P1 C1 1.908(5) . ?
P1 Sn1 2.5192(17) 5_666 ?
C1 C2 1.415(5) . ?
C1 C2 1.415(5) 2_656 ?
C1 P1 1.908(5) 2_656 ?
C2 C3 1.388(5) . ?
C2 C5 1.499(5) . ?
C3 C4 1.383(5) . ?
C3 H3A 0.9500 . ?
C4 C3 1.383(5) 2_656 ?
C4 H4A 0.9500 . ?
C5 C6 1.404(6) . ?
C5 C10 1.409(5) . ?
C6 C7 1.393(6) . ?
C6 C11 1.516(6) . ?
C7 C8 1.387(6) . ?
C7 H7A 0.9500 . ?
C8 C9 1.384(6) . ?
C8 H8A 0.9500 . ?
C9 C10 1.396(5) . ?
C9 H9A 0.9500 . ?
C10 C14 1.523(6) . ?
C11 C12 1.529(7) . ?
C11 C13 1.532(5) . ?
C11 H11A 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.483(8) . ?
C14 C15 1.500(6) . ?
C14 H14A 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.461(14) . ?
C17 C17 1.476(16) 5_766 ?
C17 H17 0.9601 . ?
C18 C19 1.510(14) . ?
C18 H18 0.9601 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
