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#$Date: 2016-03-22 11:05:44 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178884 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/13/4111356.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_4111356
loop_
_publ_author_name
'Jan J. Weigand'
'Susanne D. Riegel'
'Neil Burford'
'Andreas Decken'
_publ_contact_author_address
;Department of Chemistry
University of New Brunswick
Fredericton, NB
E3B 6E2
Canada
;
_publ_contact_author_email       adecken@unb.ca
_publ_contact_author_fax         '(506) 453-4981'
_publ_contact_author_name        'Andreas Decken'
_publ_contact_author_phone       '(506) 453-4875'
_publ_section_title
;
 Prototypical Phosphorus Analogues of Ethane: General and Versatile
 Synthetic Approaches to Hexaalkylated P-P Diphosphonium Cations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7969
_journal_page_last               7976
_journal_paper_doi               10.1021/ja071306+
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C12 H30 Cl8 Ga2 P2'
_chemical_formula_weight         659.34
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   17.749(2)
_cell_length_b                   10.2043(14)
_cell_length_c                   14.494(2)
_cell_measurement_reflns_used    7476
_cell_measurement_temperature    198(1)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.30
_cell_volume                     2625.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      198(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17073
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.29
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Kristalloflex 760'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.987
_exptl_absorpt_correction_T_max  0.6629
_exptl_absorpt_correction_T_min  0.5865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997b)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881, 2496 Friedel pairs.
;
_refine_ls_abs_structure_Flack   0.036(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         5590
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0376
_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/[σ²(Fo²)+(0.0350P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                4174
_reflns_number_total             5590
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja071306si20070411_104706.cif
_cod_data_source_block           nb060511
_cod_original_cell_volume        2625.0(6)
_cod_database_code               4111356
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
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
P1 P 0.17538(7) 0.42355(12) 0.82759(8) 0.0271(3) Uani 1 1 d .
P2 P 0.12165(6) 0.42039(12) 0.96680(9) 0.0262(3) Uani 1 1 d .
C1 C 0.2630(3) 0.5169(5) 0.8122(4) 0.0354(12) Uani 1 1 d .
C2 C 0.3185(3) 0.4865(5) 0.8899(4) 0.0423(13) Uani 1 1 d .
H2A H 0.3663 0.5318 0.8782 0.063 Uiso 1 1 calc R
H2B H 0.3274 0.3918 0.8926 0.063 Uiso 1 1 calc R
H2C H 0.2975 0.5164 0.9488 0.063 Uiso 1 1 calc R
C3 C 0.2461(3) 0.6667(5) 0.8068(4) 0.0463(14) Uani 1 1 d .
H3A H 0.2931 0.7146 0.7958 0.070 Uiso 1 1 calc R
H3B H 0.2238 0.6959 0.8652 0.070 Uiso 1 1 calc R
H3C H 0.2108 0.6837 0.7562 0.070 Uiso 1 1 calc R
C4 C 0.2953(3) 0.4738(6) 0.7184(4) 0.0464(14) Uani 1 1 d .
H4A H 0.2593 0.4952 0.6694 0.070 Uiso 1 1 calc R
H4B H 0.3043 0.3790 0.7191 0.070 Uiso 1 1 calc R
H4C H 0.3429 0.5197 0.7069 0.070 Uiso 1 1 calc R
C5 C 0.1039(3) 0.4734(5) 0.7491(4) 0.0415(13) Uani 1 1 d .
H5A H 0.1215 0.4602 0.6856 0.062 Uiso 1 1 calc R
H5B H 0.0924 0.5664 0.7587 0.062 Uiso 1 1 calc R
H5C H 0.0583 0.4212 0.7595 0.062 Uiso 1 1 calc R
C6 C 0.1945(3) 0.2535(5) 0.8049(4) 0.0442(14) Uani 1 1 d .
H6A H 0.1531 0.1998 0.8290 0.066 Uiso 1 1 calc R
H6B H 0.2417 0.2282 0.8352 0.066 Uiso 1 1 calc R
H6C H 0.1990 0.2398 0.7382 0.066 Uiso 1 1 calc R
C7 C 0.0375(3) 0.3282(5) 0.9437(3) 0.0376(12) Uani 1 1 d .
H7A H 0.0501 0.2515 0.9060 0.056 Uiso 1 1 calc R
H7B H 0.0015 0.3835 0.9104 0.056 Uiso 1 1 calc R
H7C H 0.0152 0.2994 1.0021 0.056 Uiso 1 1 calc R
C8 C 0.1786(3) 0.3229(5) 1.0422(3) 0.0391(12) Uani 1 1 d .
H8A H 0.1535 0.3144 1.1021 0.059 Uiso 1 1 calc R
H8B H 0.2277 0.3652 1.0507 0.059 Uiso 1 1 calc R
H8C H 0.1858 0.2358 1.0152 0.059 Uiso 1 1 calc R
C9 C 0.0986(2) 0.5799(4) 1.0168(3) 0.0273(10) Uani 1 1 d .
C10 C 0.0409(3) 0.5498(5) 1.0948(4) 0.0414(13) Uani 1 1 d .
H10A H 0.0611 0.4812 1.1351 0.062 Uiso 1 1 calc R
H10B H -0.0066 0.5200 1.0674 0.062 Uiso 1 1 calc R
H10C H 0.0318 0.6294 1.1310 0.062 Uiso 1 1 calc R
C11 C 0.1686(2) 0.6442(5) 1.0605(3) 0.0366(12) Uani 1 1 d .
H11A H 0.2079 0.6545 1.0135 0.055 Uiso 1 1 calc R
H11B H 0.1876 0.5886 1.1105 0.055 Uiso 1 1 calc R
H11C H 0.1550 0.7304 1.0852 0.055 Uiso 1 1 calc R
C12 C 0.0614(3) 0.6706(4) 0.9441(4) 0.0403(13) Uani 1 1 d .
H12A H 0.0444 0.7515 0.9739 0.060 Uiso 1 1 calc R
H12B H 0.0181 0.6257 0.9164 0.060 Uiso 1 1 calc R
H12C H 0.0981 0.6918 0.8959 0.060 Uiso 1 1 calc R
Ga1 Ga 0.18471(3) 0.47669(5) 0.45648(4) 0.03021(13) Uani 1 1 d .
Ga2 Ga 0.03783(3) 0.96914(5) 0.66328(4) 0.03440(14) Uani 1 1 d .
Cl1 Cl 0.13468(9) 0.49434(16) 0.32067(11) 0.0576(4) Uani 1 1 d .
Cl2 Cl 0.30627(6) 0.47277(12) 0.45019(12) 0.0411(3) Uani 1 1 d .
Cl3 Cl 0.14472(7) 0.30238(12) 0.52729(10) 0.0424(3) Uani 1 1 d .
Cl4 Cl 0.15042(6) 0.64890(12) 0.53597(9) 0.0397(3) Uani 1 1 d .
Cl5 Cl 0.15907(7) 0.95863(15) 0.67791(11) 0.0522(4) Uani 1 1 d .
Cl6 Cl -0.01509(8) 0.79209(13) 0.71730(11) 0.0555(4) Uani 1 1 d .
Cl7 Cl -0.00337(7) 1.13771(13) 0.74193(11) 0.0488(3) Uani 1 1 d .
Cl8 Cl 0.00667(9) 0.99168(13) 0.52022(11) 0.0532(4) Uani 1 1 d .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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
C5 P1 C6 107.1(3)
C5 P1 C1 112.2(2)
C6 P1 C1 108.6(2)
C5 P1 P2 106.12(19)
C6 P1 P2 103.41(18)
C1 P1 P2 118.63(17)
C8 P2 C7 107.0(2)
C8 P2 C9 112.3(2)
C7 P2 C9 110.7(2)
C8 P2 P1 108.59(18)
C7 P2 P1 101.20(17)
C9 P2 P1 116.18(16)
C2 C1 C4 110.7(4)
C2 C1 C3 111.1(4)
C4 C1 C3 107.9(4)
C2 C1 P1 110.5(3)
C4 C1 P1 105.9(3)
C3 C1 P1 110.5(3)
C1 C2 H2A 109.5
C1 C2 H2B 109.5
H2A C2 H2B 109.5
C1 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
C1 C3 H3A 109.5
C1 C3 H3B 109.5
H3A C3 H3B 109.5
C1 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
C1 C4 H4A 109.5
C1 C4 H4B 109.5
H4A C4 H4B 109.5
C1 C4 H4C 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
P1 C5 H5A 109.5
P1 C5 H5B 109.5
H5A C5 H5B 109.5
P1 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
P1 C6 H6A 109.5
P1 C6 H6B 109.5
H6A C6 H6B 109.5
P1 C6 H6C 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
P2 C7 H7A 109.5
P2 C7 H7B 109.5
H7A C7 H7B 109.5
P2 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
P2 C8 H8A 109.5
P2 C8 H8B 109.5
H8A C8 H8B 109.5
P2 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
C11 C9 C12 111.6(4)
C11 C9 C10 108.5(4)
C12 C9 C10 109.4(4)
C11 C9 P2 111.2(3)
C12 C9 P2 110.9(3)
C10 C9 P2 105.0(3)
C9 C10 H10A 109.5
C9 C10 H10B 109.5
H10A C10 H10B 109.5
C9 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
C9 C11 H11A 109.5
C9 C11 H11B 109.5
H11A C11 H11B 109.5
C9 C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
C9 C12 H12A 109.5
C9 C12 H12B 109.5
H12A C12 H12B 109.5
C9 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
Cl2 Ga1 Cl1 111.87(7)
Cl2 Ga1 Cl3 109.34(5)
Cl1 Ga1 Cl3 111.30(6)
Cl2 Ga1 Cl4 108.36(5)
Cl1 Ga1 Cl4 107.32(6)
Cl3 Ga1 Cl4 108.54(5)
Cl8 Ga2 Cl5 110.74(7)
Cl8 Ga2 Cl6 108.82(6)
Cl5 Ga2 Cl6 110.60(6)
Cl8 Ga2 Cl7 109.32(6)
Cl5 Ga2 Cl7 108.66(6)
Cl6 Ga2 Cl7 108.67(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 C5 1.779(5)
P1 C6 1.799(5)
P1 C1 1.838(5)
P1 P2 2.2320(17)
P2 C8 1.791(5)
P2 C7 1.796(4)
P2 C9 1.828(5)
C1 C2 1.528(7)
C1 C4 1.540(7)
C1 C3 1.560(7)
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
C3 H3A 0.9800
C3 H3B 0.9800
C3 H3C 0.9800
C4 H4A 0.9800
C4 H4B 0.9800
C4 H4C 0.9800
C5 H5A 0.9800
C5 H5B 0.9800
C5 H5C 0.9800
C6 H6A 0.9800
C6 H6B 0.9800
C6 H6C 0.9800
C7 H7A 0.9800
C7 H7B 0.9800
C7 H7C 0.9800
C8 H8A 0.9800
C8 H8B 0.9800
C8 H8C 0.9800
C9 C11 1.541(6)
C9 C12 1.550(6)
C9 C10 1.555(6)
C10 H10A 0.9800
C10 H10B 0.9800
C10 H10C 0.9800
C11 H11A 0.9800
C11 H11B 0.9800
C11 H11C 0.9800
C12 H12A 0.9800
C12 H12B 0.9800
C12 H12C 0.9800
Ga1 Cl2 2.1599(12)
Ga1 Cl1 2.1669(16)
Ga1 Cl3 2.1728(13)
Ga1 Cl4 2.1876(13)
Ga2 Cl8 2.1583(17)
Ga2 Cl5 2.1649(14)
Ga2 Cl6 2.1816(14)
Ga2 Cl7 2.1893(14)
