#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:48:28 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178793 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/47/4104710.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_4104710
loop_
_publ_author_name
'David V. Partyka'
'Marlena P. Washington'
'Thomas G. Gray'
'James B. Updegraff III'
'John F. Turner'
'John D. Protasiewicz'
_publ_section_title
;
 Unusual Phosphorus-Phosphorus Double Bond Contraction upon Mono- and
 Di-auration of a Diphosphene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10041
_journal_page_last               10048
_journal_paper_doi               10.1021/ja900813v
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C36 H58 Au2 Cl2 P2'
_chemical_formula_sum            'C36 H58 Au2 Cl2 P2'
_chemical_formula_weight         1017.60
_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                99.669(2)
_cell_angle_beta                 99.410(2)
_cell_angle_gamma                99.408(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8414(13)
_cell_length_b                   9.2149(14)
_cell_length_c                   12.2231(14)
_cell_measurement_reflns_used    4328
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.38
_cell_volume                     949.6(2)
_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, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker AXS APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4164
_diffrn_reflns_theta_full        27.25
_diffrn_reflns_theta_max         27.25
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.964
_exptl_absorpt_correction_T_max  0.5343
_exptl_absorpt_correction_T_min  0.3623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'AXScale in APEX2 (Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         4.938
_refine_diff_density_min         -4.697
_refine_diff_density_rms         0.354
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0717P)²+17.4751P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                3831
_reflns_number_total             4164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja900813v_si_002.cif
_cod_data_source_block           ju031908
_cod_database_code               4104710
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Au1 Au 1.24850(3) 1.25155(3) 1.07811(3) 0.01367(13) Uani 1 1 d .
P1 P 1.0715(2) 1.0678(2) 0.96622(18) 0.0115(4) Uani 1 1 d .
Cl4 Cl 1.4226(3) 1.4403(2) 1.1976(2) 0.0254(5) Uani 1 1 d .
C2 C 1.0633(9) 0.8778(9) 0.7607(7) 0.0121(15) Uani 1 1 d .
C11 C 0.7399(10) 0.7367(9) 0.4948(7) 0.0129(16) Uani 1 1 d .
C3 C 0.9728(10) 0.7941(9) 0.6592(7) 0.0147(16) Uani 1 1 d .
H3 H 1.0039 0.7058 0.6258 0.018 Uiso 1 1 calc R
C5 C 0.8055(10) 0.9679(9) 0.6507(7) 0.0136(16) Uani 1 1 d .
H5 H 0.7205 1.0007 0.6105 0.016 Uiso 1 1 calc R
C14 C 0.5672(11) 0.7136(12) 0.5047(9) 0.026(2) Uani 1 1 d .
H14A H 0.5522 0.6616 0.5669 0.039 Uiso 1 1 calc R
H14B H 0.5027 0.6531 0.4337 0.039 Uiso 1 1 calc R
H14C H 0.5364 0.8113 0.5197 0.039 Uiso 1 1 calc R
C4 C 0.8407(10) 0.8320(9) 0.6042(7) 0.0142(16) Uani 1 1 d .
C7 C 1.2164(9) 0.8218(9) 0.7987(7) 0.0130(16) Uani 1 1 d .
C1 C 1.0123(9) 1.0044(9) 0.8131(7) 0.0111(15) Uani 1 1 d .
C6 C 0.8871(9) 1.0579(9) 0.7521(7) 0.0113(15) Uani 1 1 d .
C13 C 0.7620(13) 0.8202(11) 0.3984(8) 0.024(2) Uani 1 1 d .
H13A H 0.7326 0.9183 0.4154 0.037 Uiso 1 1 calc R
H13B H 0.6957 0.7614 0.3275 0.037 Uiso 1 1 calc R
H13C H 0.8718 0.8342 0.3908 0.037 Uiso 1 1 calc R
C9 C 1.1748(11) 0.6625(11) 0.8221(9) 0.023(2) Uani 1 1 d .
H9A H 1.2704 0.6316 0.8547 0.034 Uiso 1 1 calc R
H9B H 1.1243 0.5924 0.7511 0.034 Uiso 1 1 calc R
H9C H 1.1032 0.6621 0.8755 0.034 Uiso 1 1 calc R
C16 C 0.8382(11) 1.2896(10) 0.6852(8) 0.0203(18) Uani 1 1 d .
H16A H 0.7953 1.3806 0.7017 0.030 Uiso 1 1 calc R
H16B H 0.7755 1.2246 0.6153 0.030 Uiso 1 1 calc R
H16C H 0.9465 1.3172 0.6757 0.030 Uiso 1 1 calc R
C15 C 0.8341(10) 1.2061(9) 0.7830(8) 0.0157(17) Uani 1 1 d .
C10 C 1.3076(10) 0.8173(10) 0.7014(8) 0.0175(17) Uani 1 1 d .
H10A H 1.3450 0.9199 0.6923 0.026 Uiso 1 1 calc R
H10B H 1.2387 0.7601 0.6310 0.026 Uiso 1 1 calc R
H10C H 1.3970 0.7691 0.7189 0.026 Uiso 1 1 calc R
C8 C 1.3291(11) 0.9190(11) 0.9020(8) 0.022(2) Uani 1 1 d .
H8A H 1.4279 0.8830 0.9112 0.034 Uiso 1 1 calc R
H8B H 1.2836 0.9133 0.9694 0.034 Uiso 1 1 calc R
H8C H 1.3487 1.0233 0.8921 0.034 Uiso 1 1 calc R
C12 C 0.7822(11) 0.5820(10) 0.4668(8) 0.0206(18) Uani 1 1 d .
H12A H 0.8904 0.5939 0.4555 0.031 Uiso 1 1 calc R
H12B H 0.7119 0.5233 0.3975 0.031 Uiso 1 1 calc R
H12C H 0.7713 0.5297 0.5294 0.031 Uiso 1 1 calc R
C18 C 0.9309(13) 1.3163(10) 0.8863(8) 0.025(2) Uani 1 1 d .
H18A H 1.0408 1.3343 0.8789 0.037 Uiso 1 1 calc R
H18B H 0.9212 1.2749 0.9541 0.037 Uiso 1 1 calc R
H18C H 0.8935 1.4112 0.8926 0.037 Uiso 1 1 calc R
C17 C 0.6627(12) 1.1732(11) 0.7990(10) 0.028(2) Uani 1 1 d .
H17A H 0.6334 1.2670 0.8309 0.042 Uiso 1 1 calc R
H17B H 0.6524 1.1031 0.8506 0.042 Uiso 1 1 calc R
H17C H 0.5939 1.1286 0.7256 0.042 Uiso 1 1 calc 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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
P1 Au1 Cl4 177.62(9) . .
C1 P1 P1 106.0(3) . 2_777
C1 P1 Au1 134.4(3) . .
P1 P1 Au1 119.52(16) 2_777 .
C3 C2 C1 118.0(7) . .
C3 C2 C7 113.8(7) . .
C1 C2 C7 128.1(7) . .
C4 C11 C12 112.3(7) . .
C4 C11 C13 108.4(7) . .
C12 C11 C13 109.3(7) . .
C4 C11 C14 109.8(7) . .
C12 C11 C14 108.0(7) . .
C13 C11 C14 108.9(8) . .
C4 C3 C2 123.7(8) . .
C4 C3 H3 118.2 . .
C2 C3 H3 118.2 . .
C6 C5 C4 123.8(8) . .
C6 C5 H5 118.1 . .
C4 C5 H5 118.1 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C3 C4 C5 116.6(8) . .
C3 C4 C11 123.1(8) . .
C5 C4 C11 120.2(7) . .
C8 C7 C9 108.2(8) . .
C8 C7 C10 105.7(7) . .
C9 C7 C10 109.4(7) . .
C8 C7 C2 116.2(7) . .
C9 C7 C2 109.2(7) . .
C10 C7 C2 108.0(7) . .
C2 C1 C6 119.6(7) . .
C2 C1 P1 118.8(6) . .
C6 C1 P1 119.9(6) . .
C5 C6 C1 117.3(7) . .
C5 C6 C15 114.6(7) . .
C1 C6 C15 128.0(7) . .
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 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C18 C15 C6 116.8(7) . .
C18 C15 C16 105.3(7) . .
C6 C15 C16 109.2(7) . .
C18 C15 C17 108.6(8) . .
C6 C15 C17 109.0(7) . .
C16 C15 C17 107.5(8) . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
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 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 P1 2.201(2) .
Au1 Cl4 2.250(2) .
P1 C1 1.825(9) .
P1 P1 2.003(4) 2_777
C2 C3 1.388(12) .
C2 C1 1.411(11) .
C2 C7 1.555(11) .
C11 C4 1.521(11) .
C11 C12 1.530(12) .
C11 C13 1.532(12) .
C11 C14 1.534(12) .
C3 C4 1.376(12) .
C3 H3 0.9500 .
C5 C6 1.383(12) .
C5 C4 1.391(12) .
C5 H5 0.9500 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C7 C8 1.519(12) .
C7 C9 1.540(12) .
C7 C10 1.541(12) .
C1 C6 1.434(11) .
C6 C15 1.523(11) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C16 C15 1.529(12) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C15 C18 1.513(13) .
C15 C17 1.547(13) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
