#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/44/2234490.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_2234490
loop_
_publ_author_name
'Liu, Jia-Qin'
'Zhang, Yan'
'Lü, Ya-Jing'
'Jiang, Zhen-Jü'
_publ_section_title
;
 Poly[di-μ₃-chlorido-di-μ₂-chlorido-{μ₄-N,N,N',N'-tetrakis[(diphenylphosphanyl)methyl]benzene-1,4-diamine-κ⁴P:P':P'':P'''}tetracopper(II)]
;
_journal_coeditor_code           ZQ2150
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m430
_journal_paper_doi               10.1107/S1600536812010860
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu4 Cl4 (C58 H52 N2 P4)]'
_chemical_formula_moiety         'C58 H52 Cl4 Cu4 N2 P4'
_chemical_formula_sum            'C58 H52 Cl4 Cu4 N2 P4'
_chemical_formula_weight         1296.86
_chemical_name_systematic
;
Poly[di-μ₃-chlorido-di-μ₂-chlorido-{μ₄-
N,N,N',N'-
tetrakis[(diphenylphosphanyl)methyl]benzene-1,4-diamine-
κ⁴P:P':P'':P'''}tetracopper(II)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 123.94(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.298(7)
_cell_length_b                   17.649(12)
_cell_length_c                   18.009(9)
_cell_measurement_reflns_used    5682
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.76
_cell_volume                     2715(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'ω 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  0.0853
_diffrn_reflns_av_sigmaI/netI    0.1321
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15819
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.622
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                3089
_reflns_number_total             5333
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            zq2150.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2234490
_cod_database_fobs_code          2234490
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_symmetry_multiplicity
Cu Cu1 -0.45394(8) 0.04466(4) 0.43168(4) 0.0540(2) Uani d . 1 1
Cu Cu2 -0.15464(7) 0.07255(4) 0.62081(4) 0.0487(2) Uani d . 1 1
Cl Cl1 -0.30501(14) -0.03659(7) 0.56069(8) 0.0417(3) Uani d . 1 1
Cl Cl2 -0.32846(15) 0.15805(7) 0.51454(9) 0.0526(4) Uani d . 1 1
P P1 -0.52339(15) 0.01608(8) 0.29527(8) 0.0402(3) Uani d . 1 1
P P2 -0.07631(15) -0.08176(7) 0.25371(8) 0.0367(3) Uani d . 1 1
N N1 -0.2438(4) -0.0268(2) 0.3202(2) 0.0397(10) Uani d . 1 1
C C1 -0.1055(6) 0.0562(3) 0.4500(3) 0.0370(12) Uani d . 1 1
H H1A -0.1767 0.0948 0.4172 0.044 Uiso calc R 1 1
C C2 -0.1233(5) -0.0133(3) 0.4094(3) 0.0336(11) Uani d . 1 1
C C3 -0.0155(6) -0.0698(3) 0.4619(3) 0.0364(11) Uani d . 1 1
H H3A -0.0251 -0.1175 0.4372 0.044 Uiso calc R 1 1
C C4 -0.3712(5) 0.0258(3) 0.2699(3) 0.0393(12) Uani d . 1 1
H H4A -0.4193 0.0173 0.2064 0.047 Uiso calc R 1 1
H H4B -0.3304 0.0771 0.2835 0.047 Uiso calc R 1 1
C C5 -0.5742(6) -0.0830(3) 0.2617(3) 0.0430(13) Uani d . 1 1
C C6 -0.6482(7) -0.1100(4) 0.1736(4) 0.0658(18) Uani d . 1 1
H H6A -0.6962 -0.0752 0.1269 0.079 Uiso calc R 1 1
C C7 -0.6531(8) -0.1842(4) 0.1535(5) 0.077(2) Uani d . 1 1
H H7A -0.7037 -0.1999 0.0943 0.092 Uiso calc R 1 1
C C8 -0.5818(8) -0.2361(4) 0.2222(5) 0.087(2) Uani d . 1 1
H H8A -0.5802 -0.2870 0.2094 0.104 Uiso calc R 1 1
C C9 -0.5123(8) -0.2134(4) 0.3103(4) 0.088(2) Uani d . 1 1
H H9A -0.4684 -0.2490 0.3562 0.105 Uiso calc R 1 1
C C10 -0.5089(7) -0.1380(3) 0.3292(4) 0.0647(17) Uani d . 1 1
H H10A -0.4619 -0.1230 0.3884 0.078 Uiso calc R 1 1
C C11 -0.6787(6) 0.0772(3) 0.2085(3) 0.0481(14) Uani d . 1 1
C C12 -0.7157(8) 0.0836(4) 0.1220(4) 0.078(2) Uani d . 1 1
H H12A -0.6607 0.0545 0.1053 0.094 Uiso calc R 1 1
C C13 -0.8307(9) 0.1312(4) 0.0603(4) 0.099(3) Uani d . 1 1
H H13A -0.8583 0.1319 0.0015 0.118 Uiso calc R 1 1
C C14 -0.9051(8) 0.1783(4) 0.0868(5) 0.086(2) Uani d . 1 1
H H14A -0.9836 0.2108 0.0454 0.103 Uiso calc R 1 1
C C15 -0.8645(7) 0.1776(4) 0.1730(5) 0.0743(19) Uani d . 1 1
H H15A -0.9118 0.2110 0.1910 0.089 Uiso calc R 1 1
C C16 -0.7513(7) 0.1263(3) 0.2341(4) 0.0647(17) Uani d . 1 1
H H16A -0.7245 0.1253 0.2927 0.078 Uiso calc R 1 1
C C17 -0.2353(5) -0.0931(3) 0.2727(3) 0.0402(12) Uani d . 1 1
H H17A -0.3346 -0.0990 0.2156 0.048 Uiso calc R 1 1
H H17B -0.2165 -0.1385 0.3077 0.048 Uiso calc R 1 1
C C18 -0.1096(5) -0.1626(2) 0.1820(3) 0.0352(11) Uani d . 1 1
C C19 -0.2520(6) -0.1996(3) 0.1284(3) 0.0516(14) Uani d . 1 1
H H19A -0.3385 -0.1823 0.1271 0.062 Uiso calc R 1 1
C C20 -0.2680(7) -0.2612(3) 0.0773(4) 0.0551(15) Uani d . 1 1
H H20A -0.3647 -0.2849 0.0418 0.066 Uiso calc R 1 1
C C21 -0.1420(7) -0.2879(3) 0.0785(4) 0.0525(14) Uani d . 1 1
H H21A -0.1526 -0.3296 0.0441 0.063 Uiso calc R 1 1
C C22 -0.0008(7) -0.2525(3) 0.1307(4) 0.0548(15) Uani d . 1 1
H H22A 0.0849 -0.2699 0.1312 0.066 Uiso calc R 1 1
C C23 0.0160(6) -0.1911(3) 0.1827(3) 0.0453(13) Uani d . 1 1
H H23A 0.1138 -0.1685 0.2190 0.054 Uiso calc R 1 1
C C24 -0.1553(6) 0.0012(3) 0.1797(3) 0.0430(13) Uani d . 1 1
C C25 -0.1172(7) 0.0719(3) 0.2188(4) 0.0545(15) Uani d . 1 1
H H25A -0.0423 0.0769 0.2798 0.065 Uiso calc R 1 1
C C26 -0.1918(8) 0.1364(3) 0.1661(5) 0.0701(19) Uani d . 1 1
H H26A -0.1672 0.1840 0.1928 0.084 Uiso calc R 1 1
C C27 -0.2981(8) 0.1301(4) 0.0776(4) 0.0710(19) Uani d . 1 1
H H27A -0.3477 0.1732 0.0435 0.085 Uiso calc R 1 1
C C28 -0.3334(8) 0.0610(4) 0.0378(4) 0.0714(19) Uani d . 1 1
H H28A -0.4057 0.0570 -0.0237 0.086 Uiso calc R 1 1
C C29 -0.2629(7) -0.0035(3) 0.0880(4) 0.0607(17) Uani d . 1 1
H H29A -0.2878 -0.0505 0.0599 0.073 Uiso calc R 1 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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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'
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
P1 Cu1 Cl2 . . 127.78(6)
P1 Cu1 Cl1 . . 125.05(7)
Cl2 Cu1 Cl1 . . 93.71(7)
P1 Cu1 Cl1 . 3_456 109.03(6)
Cl2 Cu1 Cl1 . 3_456 102.38(6)
Cl1 Cu1 Cl1 . 3_456 91.68(6)
P2 Cu2 Cl2 3_556 . 134.50(6)
P2 Cu2 Cl1 3_556 . 126.84(6)
Cl2 Cu2 Cl1 . . 98.57(7)
Cu2 Cl1 Cu1 . . 81.73(6)
Cu2 Cl1 Cu1 . 3_456 115.71(6)
Cu1 Cl1 Cu1 . 3_456 88.32(6)
Cu2 Cl2 Cu1 . . 82.49(7)
C5 P1 C11 . . 109.2(2)
C5 P1 C4 . . 97.5(2)
C11 P1 C4 . . 100.9(2)
C5 P1 Cu1 . . 116.30(18)
C11 P1 Cu1 . . 113.65(18)
C4 P1 Cu1 . . 117.26(16)
C18 P2 C24 . . 106.1(2)
C18 P2 C17 . . 102.1(2)
C24 P2 C17 . . 98.1(2)
C18 P2 Cu2 . 3_556 117.10(16)
C24 P2 Cu2 . 3_556 118.43(17)
C17 P2 Cu2 . 3_556 112.24(17)
C2 N1 C4 . . 121.7(4)
C2 N1 C17 . . 119.9(4)
C4 N1 C17 . . 118.2(4)
C3 C1 C2 3_556 . 121.7(4)
C3 C1 H1A 3_556 . 119.1
C2 C1 H1A . . 119.1
C1 C2 C3 . . 117.0(4)
C1 C2 N1 . . 121.9(4)
C3 C2 N1 . . 121.1(4)
C1 C3 C2 3_556 . 121.2(4)
C1 C3 H3A 3_556 . 119.4
C2 C3 H3A . . 119.4
N1 C4 P1 . . 112.3(3)
N1 C4 H4A . . 109.1
P1 C4 H4A . . 109.1
N1 C4 H4B . . 109.1
P1 C4 H4B . . 109.1
H4A C4 H4B . . 107.9
C10 C5 C6 . . 116.0(5)
C10 C5 P1 . . 117.8(4)
C6 C5 P1 . . 125.0(4)
C7 C6 C5 . . 123.2(6)
C7 C6 H6A . . 118.4
C5 C6 H6A . . 118.4
C6 C7 C8 . . 118.8(6)
C6 C7 H7A . . 120.6
C8 C7 H7A . . 120.6
C7 C8 C9 . . 120.8(6)
C7 C8 H8A . . 119.6
C9 C8 H8A . . 119.6
C10 C9 C8 . . 119.4(6)
C10 C9 H9A . . 120.3
C8 C9 H9A . . 120.3
C9 C10 C5 . . 121.7(6)
C9 C10 H10A . . 119.1
C5 C10 H10A . . 119.1
C16 C11 C12 . . 117.7(5)
C16 C11 P1 . . 117.4(4)
C12 C11 P1 . . 124.5(4)
C13 C12 C11 . . 122.2(6)
C13 C12 H12A . . 118.9
C11 C12 H12A . . 118.9
C12 C13 C14 . . 118.9(7)
C12 C13 H13A . . 120.5
C14 C13 H13A . . 120.5
C15 C14 C13 . . 120.7(6)
C15 C14 H14A . . 119.6
C13 C14 H14A . . 119.6
C14 C15 C16 . . 119.5(6)
C14 C15 H15A . . 120.2
C16 C15 H15A . . 120.2
C11 C16 C15 . . 120.8(6)
C11 C16 H16A . . 119.6
C15 C16 H16A . . 119.6
N1 C17 P2 . . 111.4(3)
N1 C17 H17A . . 109.4
P2 C17 H17A . . 109.4
N1 C17 H17B . . 109.4
P2 C17 H17B . . 109.4
H17A C17 H17B . . 108.0
C23 C18 C19 . . 117.1(4)
C23 C18 P2 . . 118.3(4)
C19 C18 P2 . . 124.6(4)
C20 C19 C18 . . 121.5(5)
C20 C19 H19A . . 119.2
C18 C19 H19A . . 119.2
C21 C20 C19 . . 120.2(5)
C21 C20 H20A . . 119.9
C19 C20 H20A . . 119.9
C22 C21 C20 . . 119.3(5)
C22 C21 H21A . . 120.3
C20 C21 H21A . . 120.3
C21 C22 C23 . . 120.6(5)
C21 C22 H22A . . 119.7
C23 C22 H22A . . 119.7
C22 C23 C18 . . 121.2(5)
C22 C23 H23A . . 119.4
C18 C23 H23A . . 119.4
C25 C24 C29 . . 118.2(5)
C25 C24 P2 . . 117.9(4)
C29 C24 P2 . . 123.6(4)
C24 C25 C26 . . 119.8(5)
C24 C25 H25A . . 120.1
C26 C25 H25A . . 120.1
C27 C26 C25 . . 120.8(5)
C27 C26 H26A . . 119.6
C25 C26 H26A . . 119.6
C26 C27 C28 . . 120.1(6)
C26 C27 H27A . . 120.0
C28 C27 H27A . . 120.0
C27 C28 C29 . . 120.5(6)
C27 C28 H28A . . 119.8
C29 C28 H28A . . 119.8
C28 C29 C24 . . 120.6(5)
C28 C29 H29A . . 119.7
C24 C29 H29A . . 119.7
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 P1 . 2.1998(19) y
Cu1 Cl2 . 2.3975(19) y
Cu1 Cl1 . 2.4140(17) y
Cu1 Cl1 3_456 2.565(2) y
Cu2 P2 3_556 2.188(2) y
Cu2 Cl2 . 2.3062(18) y
Cu2 Cl1 . 2.3255(18) y
Cl1 Cu1 3_456 2.565(2) ?
P1 C5 . 1.828(5) ?
P1 C11 . 1.837(5) ?
P1 C4 . 1.869(5) ?
P2 C18 . 1.824(5) ?
P2 C24 . 1.836(5) ?
P2 C17 . 1.861(5) ?
P2 Cu2 3_556 2.188(2) ?
N1 C2 . 1.397(5) ?
N1 C4 . 1.442(6) ?
N1 C17 . 1.479(6) ?
C1 C3 3_556 1.386(6) ?
C1 C2 . 1.387(6) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.396(6) ?
C3 C1 3_556 1.386(6) ?
C3 H3A . 0.9300 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 C10 . 1.400(7) ?
C5 C6 . 1.405(7) ?
C6 C7 . 1.352(8) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.377(9) ?
C7 H7A . 0.9300 ?
C8 C9 . 1.387(9) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.368(8) ?
C9 H9A . 0.9300 ?
C10 H10A . 0.9300 ?
C11 C16 . 1.381(7) ?
C11 C12 . 1.386(8) ?
C12 C13 . 1.369(8) ?
C12 H12A . 0.9300 ?
C13 C14 . 1.382(9) ?
C13 H13A . 0.9300 ?
C14 C15 . 1.364(9) ?
C14 H14A . 0.9300 ?
C15 C16 . 1.399(7) ?
C15 H15A . 0.9300 ?
C16 H16A . 0.9300 ?
C17 H17A . 0.9700 ?
C17 H17B . 0.9700 ?
C18 C23 . 1.381(7) ?
C18 C19 . 1.389(6) ?
C19 C20 . 1.374(7) ?
C19 H19A . 0.9300 ?
C20 C21 . 1.368(8) ?
C20 H20A . 0.9300 ?
C21 C22 . 1.364(7) ?
C21 H21A . 0.9300 ?
C22 C23 . 1.378(7) ?
C22 H22A . 0.9300 ?
C23 H23A . 0.9300 ?
C24 C25 . 1.378(7) ?
C24 C29 . 1.386(7) ?
C25 C26 . 1.404(7) ?
C25 H25A . 0.9300 ?
C26 C27 . 1.342(8) ?
C26 H26A . 0.9300 ?
C27 C28 . 1.358(8) ?
C27 H27A . 0.9300 ?
C28 C29 . 1.380(7) ?
C28 H28A . 0.9300 ?
C29 H29A . 0.9300 ?
