#------------------------------------------------------------------------------
#$Date: 2017-03-29 19:04:36 +0300 (Wed, 29 Mar 2017) $
#$Revision: 194596 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/19/2201990.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_2201990
loop_
_publ_author_name
'Wu, Mei-Mei'
'Zhang, Li-Yi'
'Qin, Yong-Hai'
'Chen, Zhong-Ning'
_publ_section_title
;Bis[μ-bis(diphenylphosphino)methane-κ²P:P']bis[diacetonitrilecopper(I)]
 bis(hexafluorophosphate)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m195
_journal_page_last               m196
_journal_paper_doi               10.1107/S1600536803006330
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cu2 (C25 H22 P2)2 (C2 H3 N)4] (P F6)2'
_chemical_formula_moiety         'C58 H56 Cu2 N4 P4 2+, 2P F6 1-'
_chemical_formula_sum            'C58 H56 Cu2 F12 N4 P6'
_chemical_formula_weight         1349.97
_chemical_name_common            'Cu2 P6 F12 C58 H56 N4'
_chemical_name_systematic
;
Bis[μ-bis(diphenylphosphino)methane-κ²P:P']bis[diacetonitrilecopper(I)]
bis(hexafluorophosphate)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 108.7480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.5125(3)
_cell_length_b                   13.1916(2)
_cell_length_c                   21.6096(3)
_cell_measurement_reflns_used    4793
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.82
_cell_volume                     6077.02(15)
_computing_cell_refinement       'SMART and SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'XPREP in SHELXTL (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Siemens SMART 1K CCD'
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8897
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  .592
_exptl_absorpt_correction_T_min  .561
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          .60
_exptl_crystal_size_mid          .56
_exptl_crystal_size_min          .56
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.663
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0679
_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)+(0.0384P)²+40.8701P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                4180
_reflns_number_total             5273
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fl6025.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Replacing the "\K" substring with the "\k" substring in the
 _chemical_name_systematic data item value.

 Antanas Vaitkus,
 2017-03-29
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2201990
_cod_database_fobs_code          2201990
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'
'-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_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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu1 0.44474(3) 0.64257(5) 0.79918(3) 0.0433(2) Uani d . 1 . . Cu
P1 0.38179(6) 0.70275(11) 0.70157(6) 0.0372(3) Uani d . 1 . . P
P2 0.51986(6) 0.74477(11) 0.86682(6) 0.0369(3) Uani d . 1 . . P
P3 0.12445(10) 0.37859(16) 0.37166(10) 0.0678(5) Uani d . 1 . . P
F1 0.0778(4) 0.4279(7) 0.3144(4) 0.192(4) Uani d . 1 . . F
F2 0.1679(5) 0.3197(6) 0.4271(4) 0.195(4) Uani d . 1 . . F
F3 0.1111(4) 0.2824(8) 0.3281(4) 0.195(4) Uani d . 1 . . F
F4 0.0766(5) 0.3449(8) 0.4021(5) 0.215(5) Uani d . 1 . . F
F5 0.1805(4) 0.3977(7) 0.3503(5) 0.205(4) Uani d . 1 . . F
F6 0.1347(4) 0.4777(5) 0.4096(4) 0.151(2) Uani d . 1 . . F
N1 0.4595(2) 0.4906(4) 0.8079(2) 0.0552(13) Uani d . 1 . . N
N2 0.3827(3) 0.6485(4) 0.8580(3) 0.0595(14) Uani d . 1 . . N
C1 0.4631(3) 0.4063(5) 0.8172(3) 0.0591(16) Uani d . 1 . . C
C01 0.5831(2) 0.7964(4) 0.8396(3) 0.0382(12) Uani d . 1 . . C
H01A 0.6156 0.8233 0.8772 0.046 Uiso calc R 1 . . H
H01B 0.5665 0.8523 0.8098 0.046 Uiso calc R 1 . . H
C2 0.4661(6) 0.2965(6) 0.8286(7) 0.107(3) Uani d . 1 . . C
HC2A 0.5044 0.2800 0.8625 0.19(6) Uiso calc R 1 . . H
HC2B 0.4648 0.2619 0.7891 0.19(6) Uiso calc R 1 . . H
HC2C 0.4310 0.2757 0.8417 0.22(7) Uiso calc R 1 . . H
C3 0.3533(3) 0.6836(6) 0.8851(3) 0.0654(18) Uani d . 1 . . C
C4 0.3146(5) 0.7325(8) 0.9196(5) 0.108(3) Uiso d . 1 . . C
H4A 0.3287 0.7120 0.9646 0.162 Uiso calc R 1 . . H
H4B 0.2716 0.7127 0.8998 0.162 Uiso calc R 1 . . H
H4C 0.3181 0.8047 0.9169 0.162 Uiso calc R 1 . . H
C111 0.3414(3) 0.6132(4) 0.6372(3) 0.0443(13) Uani d . 1 . . C
C112 0.3575(3) 0.5117(5) 0.6433(3) 0.0554(15) Uani d . 1 . . C
H11A 0.3900 0.4894 0.6794 0.066 Uiso calc R 1 . . H
C113 0.3253(4) 0.4426(6) 0.5957(4) 0.077(2) Uani d . 1 . . C
H11C 0.3368 0.3746 0.5997 0.092 Uiso calc R 1 . . H
C114 0.2765(4) 0.4746(7) 0.5429(4) 0.078(2) Uani d . 1 . . C
H11D 0.2539 0.4280 0.5120 0.093 Uiso calc R 1 . . H
C115 0.2611(3) 0.5749(6) 0.5356(3) 0.075(2) Uani d . 1 . . C
H11E 0.2288 0.5965 0.4990 0.090 Uiso calc R 1 . . H
C116 0.2931(3) 0.6445(5) 0.5822(3) 0.0623(17) Uani d . 1 . . C
H11B 0.2822 0.7127 0.5768 0.075 Uiso calc R 1 . . H
C121 0.3159(3) 0.7721(5) 0.7137(3) 0.0454(13) Uani d . 1 . . C
C122 0.3127(3) 0.8763(6) 0.7142(4) 0.072(2) Uani d . 1 . . C
H12B 0.3434 0.9147 0.7048 0.087 Uiso calc R 1 . . H
C123 0.2636(4) 0.9246(8) 0.7287(5) 0.103(3) Uani d . 1 . . C
H12E 0.2611 0.9949 0.7281 0.123 Uiso calc R 1 . . H
C124 0.2189(4) 0.8675(10) 0.7439(4) 0.101(4) Uani d . 1 . . C
H12C 0.1872 0.8997 0.7555 0.122 Uiso calc R 1 . . H
C125 0.2207(4) 0.7638(10) 0.7420(4) 0.095(3) Uani d . 1 . . C
H12D 0.1896 0.7256 0.7509 0.114 Uiso calc R 1 . . H
C126 0.2687(3) 0.7165(6) 0.7268(3) 0.0671(19) Uani d . 1 . . C
H12A 0.2697 0.6461 0.7253 0.080 Uiso calc R 1 . . H
C211 0.5619(2) 0.6938(4) 0.9477(2) 0.0430(13) Uani d . 1 . . C
C212 0.6053(3) 0.7506(6) 0.9957(3) 0.0611(17) Uani d . 1 . . C
H21D 0.6124 0.8181 0.9879 0.073 Uiso calc R 1 . . H
C213 0.6377(3) 0.7063(7) 1.0550(3) 0.073(2) Uani d . 1 . . C
H21B 0.6664 0.7447 1.0870 0.088 Uiso calc R 1 . . H
C214 0.6282(4) 0.6065(7) 1.0673(3) 0.080(2) Uani d . 1 . . C
H21C 0.6505 0.5776 1.1073 0.097 Uiso calc R 1 . . H
C215 0.5858(4) 0.5499(6) 1.0206(3) 0.081(2) Uani d . 1 . . C
H21E 0.5790 0.4824 1.0287 0.097 Uiso calc R 1 . . H
C216 0.5526(3) 0.5936(5) 0.9608(3) 0.0616(17) Uani d . 1 . . C
H21A 0.5239 0.5547 0.9292 0.074 Uiso calc R 1 . . H
C221 0.4813(2) 0.8582(4) 0.8845(3) 0.0425(12) Uani d . 1 . . C
C222 0.4621(3) 0.9350(5) 0.8384(3) 0.0555(15) Uani d . 1 . . C
H22A 0.4744 0.9328 0.8012 0.067 Uiso calc R 1 . . H
C223 0.4252(4) 1.0146(5) 0.8464(4) 0.077(2) Uani d . 1 . . C
H22E 0.4128 1.0651 0.8148 0.093 Uiso calc R 1 . . H
C224 0.4072(4) 1.0188(6) 0.9006(4) 0.083(2) Uani d . 1 . . C
H22D 0.3818 1.0715 0.9057 0.100 Uiso calc R 1 . . H
C225 0.4263(4) 0.9457(7) 0.9479(4) 0.083(2) Uani d . 1 . . C
H22C 0.4149 0.9502 0.9855 0.100 Uiso calc R 1 . . H
C226 0.4628(3) 0.8647(6) 0.9401(3) 0.0641(18) Uani d . 1 . . C
H22B 0.4750 0.8147 0.9720 0.077 Uiso calc R 1 . . H
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'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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
N1 Cu1 N2 . . 95.6(2) yes
N1 Cu1 P1 . . 117.74(14) yes
N2 Cu1 P1 . . 101.79(14) yes
N1 Cu1 P2 . . 117.24(15) yes
N2 Cu1 P2 . . 95.01(15) yes
P1 Cu1 P2 . . 119.99(6) yes
C111 P1 C121 . . 101.7(3) ?
C111 P1 C01 . 2_656 104.6(2) ?
C121 P1 C01 . 2_656 103.1(3) ?
C111 P1 Cu1 . . 119.29(19) ?
C121 P1 Cu1 . . 109.52(17) yes
C01 P1 Cu1 2_656 . 116.46(18) yes
C211 P2 C221 . . 103.6(3) ?
C211 P2 C01 . . 103.1(2) ?
C221 P2 C01 . . 103.4(2) ?
C211 P2 Cu1 . . 116.35(19) yes
C221 P2 Cu1 . . 108.21(17) ?
C01 P2 Cu1 . . 120.26(17) yes
F1 P3 F2 . . 174.5(5) ?
F1 P3 F5 . . 96.2(6) ?
F2 P3 F5 . . 86.3(6) ?
F1 P3 F4 . . 94.6(6) ?
F2 P3 F4 . . 82.7(6) ?
F5 P3 F4 . . 168.8(6) ?
F1 P3 F6 . . 91.0(5) ?
F2 P3 F6 . . 93.9(4) ?
F5 P3 F6 . . 91.5(5) ?
F4 P3 F6 . . 91.3(5) ?
F1 P3 F3 . . 84.6(5) ?
F2 P3 F3 . . 90.6(5) ?
F5 P3 F3 . . 88.2(5) ?
F4 P3 F3 . . 89.9(5) ?
F6 P3 F3 . . 175.5(5) ?
C1 N1 Cu1 . . 171.8(6) yes
C3 N2 Cu1 . . 157.5(6) yes
N1 C1 C2 . . 178.5(9) ?
P2 C01 P1 . 2_656 113.8(3) ?
P2 C01 H01A . . 108.8 ?
P1 C01 H01A 2_656 . 108.8 ?
P2 C01 H01B . . 108.8 ?
P1 C01 H01B 2_656 . 108.8 ?
H01A C01 H01B . . 107.7 ?
C1 C2 HC2A . . 109.5 ?
C1 C2 HC2B . . 109.5 ?
HC2A C2 HC2B . . 109.5 ?
C1 C2 HC2C . . 109.5 ?
HC2A C2 HC2C . . 109.5 ?
HC2B C2 HC2C . . 109.5 ?
N2 C3 C4 . . 178.3(9) ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
C112 C111 C116 . . 118.5(5) ?
C112 C111 P1 . . 120.2(4) ?
C116 C111 P1 . . 121.3(5) ?
C111 C112 C113 . . 120.5(6) ?
C111 C112 H11A . . 119.8 ?
C113 C112 H11A . . 119.8 ?
C114 C113 C112 . . 120.0(7) ?
C114 C113 H11C . . 120.0 ?
C112 C113 H11C . . 120.0 ?
C115 C114 C113 . . 120.1(7) ?
C115 C114 H11D . . 120.0 ?
C113 C114 H11D . . 120.0 ?
C114 C115 C116 . . 120.4(7) ?
C114 C115 H11E . . 119.8 ?
C116 C115 H11E . . 119.8 ?
C115 C116 C111 . . 120.5(6) ?
C115 C116 H11B . . 119.8 ?
C111 C116 H11B . . 119.8 ?
C122 C121 C126 . . 118.6(6) ?
C122 C121 P1 . . 123.2(5) ?
C126 C121 P1 . . 118.1(5) ?
C121 C122 C123 . . 120.3(8) ?
C121 C122 H12B . . 119.8 ?
C123 C122 H12B . . 119.8 ?
C124 C123 C122 . . 119.7(9) ?
C124 C123 H12E . . 120.1 ?
C122 C123 H12E . . 120.1 ?
C125 C124 C123 . . 120.5(8) ?
C125 C124 H12C . . 119.8 ?
C123 C124 H12C . . 119.8 ?
C124 C125 C126 . . 119.5(9) ?
C124 C125 H12D . . 120.2 ?
C126 C125 H12D . . 120.2 ?
C125 C126 C121 . . 121.2(8) ?
C125 C126 H12A . . 119.4 ?
C121 C126 H12A . . 119.4 ?
C216 C211 C212 . . 118.6(6) ?
C216 C211 P2 . . 118.8(4) ?
C212 C211 P2 . . 122.6(5) ?
C213 C212 C211 . . 119.9(7) ?
C213 C212 H21D . . 120.1 ?
C211 C212 H21D . . 120.1 ?
C214 C213 C212 . . 121.0(7) ?
C214 C213 H21B . . 119.5 ?
C212 C213 H21B . . 119.5 ?
C215 C214 C213 . . 119.7(7) ?
C215 C214 H21C . . 120.2 ?
C213 C214 H21C . . 120.2 ?
C214 C215 C216 . . 119.9(7) ?
C214 C215 H21E . . 120.1 ?
C216 C215 H21E . . 120.1 ?
C211 C216 C215 . . 121.0(6) ?
C211 C216 H21A . . 119.5 ?
C215 C216 H21A . . 119.5 ?
C222 C221 C226 . . 117.7(6) ?
C222 C221 P2 . . 120.3(4) ?
C226 C221 P2 . . 121.5(5) ?
C223 C222 C221 . . 121.6(6) ?
C223 C222 H22A . . 119.2 ?
C221 C222 H22A . . 119.2 ?
C224 C223 C222 . . 119.7(7) ?
C224 C223 H22E . . 120.1 ?
C222 C223 H22E . . 120.1 ?
C223 C224 C225 . . 120.4(7) ?
C223 C224 H22D . . 119.8 ?
C225 C224 H22D . . 119.8 ?
C224 C225 C226 . . 120.3(7) ?
C224 C225 H22C . . 119.8 ?
C226 C225 H22C . . 119.8 ?
C225 C226 C221 . . 120.3(7) ?
C225 C226 H22B . . 119.9 ?
C221 C226 H22B . . 119.9 ?
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
Cu1 N1 . 2.031(5) yes
Cu1 N2 . 2.172(6) yes
Cu1 P1 . 2.2730(14) yes
Cu1 P2 . 2.2859(15) yes
P1 C111 . 1.829(5) ?
P1 C121 . 1.832(6) ?
P1 C01 2_656 1.843(5) ?
P2 C211 . 1.828(5) ?
P2 C221 . 1.831(6) ?
P2 C01 . 1.837(5) ?
P3 F1 . 1.490(7) ?
P3 F2 . 1.497(8) ?
P3 F5 . 1.498(9) ?
P3 F4 . 1.499(8) ?
P3 F6 . 1.521(7) ?
P3 F3 . 1.551(9) ?
N1 C1 . 1.128(8) ?
N2 C3 . 1.115(8) ?
C1 C2 . 1.468(10) ?
C01 P1 2_656 1.843(5) ?
C01 H01A . 0.9700 ?
C01 H01B . 0.9700 ?
C2 HC2A . 0.9600 ?
C2 HC2B . 0.9600 ?
C2 HC2C . 0.9600 ?
C3 C4 . 1.465(11) ?
C4 H4A . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
C111 C112 . 1.382(8) ?
C111 C116 . 1.391(8) ?
C112 C113 . 1.391(9) ?
C112 H11A . 0.9300 ?
C113 C114 . 1.372(11) ?
C113 H11C . 0.9300 ?
C114 C115 . 1.363(11) ?
C114 H11D . 0.9300 ?
C115 C116 . 1.383(9) ?
C115 H11E . 0.9300 ?
C116 H11B . 0.9300 ?
C121 C122 . 1.376(9) ?
C121 C126 . 1.394(8) ?
C122 C123 . 1.396(10) ?
C122 H12B . 0.9300 ?
C123 C124 . 1.380(14) ?
C123 H12E . 0.9300 ?
C124 C125 . 1.369(14) ?
C124 H12C . 0.9300 ?
C125 C126 . 1.377(11) ?
C125 H12D . 0.9300 ?
C126 H12A . 0.9300 ?
C211 C216 . 1.381(8) ?
C211 C212 . 1.393(8) ?
C212 C213 . 1.383(9) ?
C212 H21D . 0.9300 ?
C213 C214 . 1.374(11) ?
C213 H21B . 0.9300 ?
C214 C215 . 1.368(11) ?
C214 H21C . 0.9300 ?
C215 C216 . 1.392(9) ?
C215 H21E . 0.9300 ?
C216 H21A . 0.9300 ?
C221 C222 . 1.389(8) ?
C221 C226 . 1.393(8) ?
C222 C223 . 1.385(9) ?
C222 H22A . 0.9300 ?
C223 C224 . 1.359(11) ?
C223 H22E . 0.9300 ?
C224 C225 . 1.370(11) ?
C224 H22D . 0.9300 ?
C225 C226 . 1.391(10) ?
C225 H22C . 0.9300 ?
C226 H22B . 0.9300 ?
