#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/04/2210499.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2210499
loop_
_publ_author_name
'Cao, Qian-Yong'
'Yin, Bei'
'Liu, Jing-Hua'
_publ_section_title
;
 Bis[μ-bis(diphenylphosphino)methane-κ²P:P']digold(I)
 bis(perchlorate)
;
_journal_coeditor_code           BH2047
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2730
_journal_page_last               m2731
_journal_paper_doi               10.1107/S1600536806038542
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Au2 (C25 H22 P2)2] (Cl O4)2'
_chemical_formula_moiety         'C50 H44 Au2 P4 2+, 2Cl O4 -'
_chemical_formula_sum            'C50 H44 Au2 Cl2 O8 P4'
_chemical_formula_weight         1361.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.287(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.569(4)
_cell_length_b                   17.648(6)
_cell_length_c                   13.797(5)
_cell_measurement_reflns_used    963
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      3.39
_cell_volume                     2482.4(16)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13943
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.192
_exptl_absorpt_correction_T_max  0.420
_exptl_absorpt_correction_T_min  0.225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.556
_refine_diff_density_min         -1.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5069
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0377
_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)+(0.0322P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                3681
_reflns_number_total             5069
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bh2047.cif
_cod_data_source_block           I
_cod_original_cell_volume        2482.3(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2210499
_cod_database_fobs_code          2210499
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Au Au1 0.381797(18) 0.491529(13) 0.535251(15) 0.03472(9) Uani d . 1
P P1 0.49059(13) 0.41547(9) 0.66767(10) 0.0326(3) Uani d . 1
P P2 0.73575(13) 0.43238(9) 0.59365(10) 0.0316(3) Uani d . 1
C C1 0.3882(5) 0.3423(4) 0.6988(4) 0.0378(14) Uani d . 1
C C2 0.2929(6) 0.3651(5) 0.7464(5) 0.062(2) Uani d . 1
H H2 0.2864 0.4157 0.7632 0.075 Uiso calc R 1
C C3 0.2088(7) 0.3120(5) 0.7681(6) 0.071(2) Uani d . 1
H H3 0.1475 0.3269 0.8020 0.085 Uiso calc R 1
C C4 0.2138(7) 0.2381(5) 0.7409(6) 0.072(2) Uani d . 1
H H4 0.1545 0.2033 0.7544 0.087 Uiso calc R 1
C C5 0.3064(7) 0.2148(5) 0.6936(6) 0.076(2) Uani d . 1
H H5 0.3116 0.1643 0.6761 0.092 Uiso calc R 1
C C6 0.3912(6) 0.2676(4) 0.6728(5) 0.0582(19) Uani d . 1
H H6 0.4529 0.2519 0.6398 0.070 Uiso calc R 1
C C7 0.5522(5) 0.4672(4) 0.7834(4) 0.0413(15) Uani d . 1
C C8 0.6168(6) 0.4303(4) 0.8707(5) 0.0578(19) Uani d . 1
H H8 0.6294 0.3782 0.8703 0.069 Uiso calc R 1
C C9 0.6628(8) 0.4713(6) 0.9590(5) 0.077(2) Uani d . 1
H H9 0.7057 0.4464 1.0179 0.093 Uiso calc R 1
C C10 0.6451(8) 0.5480(6) 0.9594(6) 0.085(3) Uani d . 1
H H10 0.6763 0.5750 1.0188 0.102 Uiso calc R 1
C C11 0.5824(9) 0.5853(6) 0.8739(7) 0.098(3) Uani d . 1
H H11 0.5714 0.6376 0.8746 0.117 Uiso calc R 1
C C12 0.5350(8) 0.5445(5) 0.7857(5) 0.070(2) Uani d . 1
H H12 0.4912 0.5697 0.7273 0.084 Uiso calc R 1
C C13 0.6312(5) 0.3677(3) 0.6410(4) 0.0342(13) Uani d . 1
H H13A 0.6829 0.3439 0.7020 0.041 Uiso calc R 1
H H13B 0.5998 0.3282 0.5917 0.041 Uiso calc R 1
C C14 0.8303(5) 0.4850(3) 0.7005(4) 0.0356(13) Uani d . 1
C C15 0.9178(6) 0.4482(4) 0.7795(4) 0.0468(16) Uani d . 1
H H15 0.9297 0.3961 0.7772 0.056 Uiso calc R 1
C C16 0.9870(7) 0.4894(5) 0.8614(5) 0.065(2) Uani d . 1
H H16 1.0461 0.4647 0.9139 0.078 Uiso calc R 1
C C17 0.9700(7) 0.5653(5) 0.8665(6) 0.073(2) Uani d . 1
H H17 1.0175 0.5925 0.9220 0.087 Uiso calc R 1
C C18 0.8821(8) 0.6019(5) 0.7893(6) 0.081(3) Uani d . 1
H H18 0.8692 0.6538 0.7932 0.098 Uiso calc R 1
C C19 0.8130(6) 0.5621(4) 0.7062(5) 0.0590(19) Uani d . 1
H H19 0.7546 0.5874 0.6538 0.071 Uiso calc R 1
C C20 0.8534(5) 0.3739(3) 0.5529(4) 0.0333(13) Uani d . 1
C C21 0.8324(6) 0.3019(4) 0.5222(5) 0.0578(19) Uani d . 1
H H21 0.7560 0.2774 0.5263 0.069 Uiso calc R 1
C C22 0.9242(7) 0.2632(4) 0.4842(6) 0.067(2) Uani d . 1
H H22 0.9082 0.2132 0.4635 0.081 Uiso calc R 1
C C23 1.0336(7) 0.2965(5) 0.4771(5) 0.062(2) Uani d . 1
H H23 1.0917 0.2710 0.4485 0.074 Uiso calc R 1
C C24 1.0600(7) 0.3675(6) 0.5117(6) 0.078(3) Uani d . 1
H H24 1.1393 0.3899 0.5105 0.093 Uiso calc R 1
C C25 0.9702(7) 0.4079(5) 0.5492(6) 0.071(2) Uani d . 1
H H25 0.9885 0.4574 0.5717 0.086 Uiso calc R 1
Cl Cl1 0.41267(16) 0.25816(11) 0.39094(13) 0.0538(4) Uani d . 1
O O1 0.4043(7) 0.2524(4) 0.2890(4) 0.127(3) Uani d U 1
O O2 0.5068(6) 0.2081(3) 0.4466(4) 0.0980(19) Uani d U 1
O O3 0.4355(9) 0.3289(4) 0.4279(5) 0.195(5) Uani d U 1
O O4 0.2931(7) 0.2368(7) 0.3976(8) 0.213(5) Uani d U 1
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'
O O 0.0106 0.0060 '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'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P2 Au1 P1 3_666 . 177.14(5) yes
P2 Au1 Au1 3_666 3_666 91.02(4) yes
P1 Au1 Au1 . 3_666 91.81(4) yes
C7 P1 C1 . . 104.5(3) ?
C7 P1 C13 . . 106.8(3) ?
C1 P1 C13 . . 106.7(3) ?
C7 P1 Au1 . . 113.1(2) ?
C1 P1 Au1 . . 113.44(18) ?
C13 P1 Au1 . . 111.69(18) ?
C14 P2 C20 . . 105.6(3) ?
C14 P2 C13 . . 106.7(3) ?
C20 P2 C13 . . 106.5(3) ?
C14 P2 Au1 . 3_666 113.5(2) ?
C20 P2 Au1 . 3_666 111.43(18) ?
C13 P2 Au1 . 3_666 112.67(17) ?
C6 C1 C2 . . 117.9(6) ?
C6 C1 P1 . . 124.7(5) ?
C2 C1 P1 . . 117.2(5) ?
C3 C2 C1 . . 119.5(7) ?
C3 C2 H2 . . 120.2 ?
C1 C2 H2 . . 120.2 ?
C4 C3 C2 . . 121.1(7) ?
C4 C3 H3 . . 119.5 ?
C2 C3 H3 . . 119.5 ?
C3 C4 C5 . . 120.1(8) ?
C3 C4 H4 . . 119.9 ?
C5 C4 H4 . . 119.9 ?
C4 C5 C6 . . 118.8(8) ?
C4 C5 H5 . . 120.6 ?
C6 C5 H5 . . 120.6 ?
C1 C6 C5 . . 122.4(6) ?
C1 C6 H6 . . 118.8 ?
C5 C6 H6 . . 118.8 ?
C12 C7 C8 . . 119.0(6) ?
C12 C7 P1 . . 120.2(5) ?
C8 C7 P1 . . 120.8(6) ?
C7 C8 C9 . . 119.8(8) ?
C7 C8 H8 . . 120.1 ?
C9 C8 H8 . . 120.1 ?
C10 C9 C8 . . 120.2(8) ?
C10 C9 H9 . . 119.9 ?
C8 C9 H9 . . 119.9 ?
C11 C10 C9 . . 120.7(8) ?
C11 C10 H10 . . 119.6 ?
C9 C10 H10 . . 119.6 ?
C10 C11 C12 . . 119.3(9) ?
C10 C11 H11 . . 120.3 ?
C12 C11 H11 . . 120.3 ?
C7 C12 C11 . . 120.9(7) ?
C7 C12 H12 . . 119.5 ?
C11 C12 H12 . . 119.5 ?
P2 C13 P1 . . 112.6(3) ?
P2 C13 H13A . . 109.1 ?
P1 C13 H13A . . 109.1 ?
P2 C13 H13B . . 109.1 ?
P1 C13 H13B . . 109.1 ?
H13A C13 H13B . . 107.8 ?
C19 C14 C15 . . 119.2(5) ?
C19 C14 P2 . . 120.1(4) ?
C15 C14 P2 . . 120.7(5) ?
C16 C15 C14 . . 119.7(6) ?
C16 C15 H15 . . 120.2 ?
C14 C15 H15 . . 120.2 ?
C17 C16 C15 . . 121.0(7) ?
C17 C16 H16 . . 119.5 ?
C15 C16 H16 . . 119.5 ?
C16 C17 C18 . . 119.7(7) ?
C16 C17 H17 . . 120.2 ?
C18 C17 H17 . . 120.2 ?
C17 C18 C19 . . 120.4(8) ?
C17 C18 H18 . . 119.8 ?
C19 C18 H18 . . 119.8 ?
C18 C19 C14 . . 120.1(7) ?
C18 C19 H19 . . 120.0 ?
C14 C19 H19 . . 120.0 ?
C21 C20 C25 . . 118.3(6) ?
C21 C20 P2 . . 124.6(5) ?
C25 C20 P2 . . 117.0(5) ?
C20 C21 C22 . . 120.6(6) ?
C20 C21 H21 . . 119.7 ?
C22 C21 H21 . . 119.7 ?
C23 C22 C21 . . 121.2(7) ?
C23 C22 H22 . . 119.4 ?
C21 C22 H22 . . 119.4 ?
C22 C23 C24 . . 119.5(7) ?
C22 C23 H23 . . 120.3 ?
C24 C23 H23 . . 120.3 ?
C23 C24 C25 . . 120.8(7) ?
C23 C24 H24 . . 119.6 ?
C25 C24 H24 . . 119.6 ?
C20 C25 C24 . . 119.5(7) ?
C20 C25 H25 . . 120.2 ?
C24 C25 H25 . . 120.2 ?
O4 Cl1 O3 . . 108.2(7) ?
O4 Cl1 O1 . . 103.8(5) ?
O3 Cl1 O1 . . 114.1(5) ?
O4 Cl1 O2 . . 109.3(6) ?
O3 Cl1 O2 . . 110.3(4) ?
O1 Cl1 O2 . . 110.8(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Au1 P2 3_666 2.3118(15) yes
Au1 P1 . 2.3138(15) yes
Au1 Au1 3_666 2.9258(9) yes
P1 C7 . 1.805(6) ?
P1 C1 . 1.807(6) ?
P1 C13 . 1.829(5) ?
P2 C14 . 1.805(6) ?
P2 C20 . 1.815(6) ?
P2 C13 . 1.825(5) ?
P2 Au1 3_666 2.3118(15) ?
C1 C6 . 1.370(9) ?
C1 C2 . 1.399(8) ?
C2 C3 . 1.379(9) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.362(11) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.374(10) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.375(9) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C12 . 1.376(10) ?
C7 C8 . 1.381(8) ?
C8 C9 . 1.390(10) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.367(14) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.361(11) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.390(10) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C14 C19 . 1.378(9) ?
C14 C15 . 1.392(8) ?
C15 C16 . 1.379(9) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.355(10) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.377(10) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.378(9) ?
C18 H18 . 0.9300 ?
C19 H19 . 0.9300 ?
C20 C21 . 1.339(9) ?
C20 C25 . 1.387(8) ?
C21 C22 . 1.397(9) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.323(10) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.343(11) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.392(10) ?
C24 H24 . 0.9300 ?
C25 H25 . 0.9300 ?
Cl1 O4 . 1.345(6) ?
Cl1 O3 . 1.346(6) ?
Cl1 O1 . 1.389(6) ?
Cl1 O2 . 1.399(5) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
Au1 Au1 P1 C7 3_666 95.6(2)
Au1 Au1 P1 C1 3_666 -145.6(2)
Au1 Au1 P1 C13 3_666 -24.9(2)
C7 P1 C1 C6 . -133.6(6)
C13 P1 C1 C6 . -20.7(6)
Au1 P1 C1 C6 . 102.8(5)
C7 P1 C1 C2 . 51.3(5)
C13 P1 C1 C2 . 164.2(5)
Au1 P1 C1 C2 . -72.4(5)
C6 C1 C2 C3 . 2.0(10)
P1 C1 C2 C3 . 177.4(5)
C1 C2 C3 C4 . -2.3(12)
C2 C3 C4 C5 . 2.0(13)
C3 C4 C5 C6 . -1.3(12)
C2 C1 C6 C5 . -1.3(10)
P1 C1 C6 C5 . -176.4(6)
C4 C5 C6 C1 . 1.0(12)
C1 P1 C7 C12 . -125.5(6)
C13 P1 C7 C12 . 121.7(5)
Au1 P1 C7 C12 . -1.6(6)
C1 P1 C7 C8 . 54.5(5)
C13 P1 C7 C8 . -58.4(5)
Au1 P1 C7 C8 . 178.4(4)
C12 C7 C8 C9 . 0.3(10)
P1 C7 C8 C9 . -179.7(5)
C7 C8 C9 C10 . -0.5(11)
C8 C9 C10 C11 . 0.1(13)
C9 C10 C11 C12 . 0.6(14)
C8 C7 C12 C11 . 0.4(11)
P1 C7 C12 C11 . -179.7(6)
C10 C11 C12 C7 . -0.8(13)
C14 P2 C13 P1 . 76.4(3)
C20 P2 C13 P1 . -171.2(3)
Au1 P2 C13 P1 3_666 -48.7(3)
C7 P1 C13 P2 . -75.5(4)
C1 P1 C13 P2 . 173.2(3)
Au1 P1 C13 P2 . 48.7(3)
C20 P2 C14 C19 . 131.9(5)
C13 P2 C14 C19 . -115.1(5)
Au1 P2 C14 C19 3_666 9.6(6)
C20 P2 C14 C15 . -50.4(5)
C13 P2 C14 C15 . 62.6(5)
Au1 P2 C14 C15 3_666 -172.7(4)
C19 C14 C15 C16 . -0.9(9)
P2 C14 C15 C16 . -178.6(5)
C14 C15 C16 C17 . 0.6(11)
C15 C16 C17 C18 . 0.3(12)
C16 C17 C18 C19 . -1.1(12)
C17 C18 C19 C14 . 0.8(12)
C15 C14 C19 C18 . 0.1(10)
P2 C14 C19 C18 . 177.9(6)
C14 P2 C20 C21 . 139.6(6)
C13 P2 C20 C21 . 26.5(6)
Au1 P2 C20 C21 3_666 -96.7(6)
C14 P2 C20 C25 . -43.6(6)
C13 P2 C20 C25 . -156.7(5)
Au1 P2 C20 C25 3_666 80.1(5)
C25 C20 C21 C22 . -2.2(10)
P2 C20 C21 C22 . 174.6(5)
C20 C21 C22 C23 . -0.3(12)
C21 C22 C23 C24 . 3.3(13)
C22 C23 C24 C25 . -3.9(13)
C21 C20 C25 C24 . 1.6(11)
P2 C20 C25 C24 . -175.4(6)
C23 C24 C25 C20 . 1.4(13)
