#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/78/7027829.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7027829
loop_
_publ_author_name
'Ainscough, Eric W.'
'Brodie, Andrew M.'
'Depree, Craig V.'
_publ_section_title
;
 Polymer building blocks: a CuCl2-bridged phosphazene dimer containing
 κ5N coordinated Cu(II) †
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4123
_journal_paper_doi               10.1039/a908430d
_journal_year                    1999
_chemical_formula_moiety         C60H48N18O12P6Cl10Cu5
_chemical_formula_sum            'C30 H24 Cl5 Cu2.5 N9 O6 P3'
_chemical_formula_weight         1035.59
_chemical_name_systematic
; 
 ? 
;
_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                 114.145(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.205(6)
_cell_length_b                   20.141(4)
_cell_length_c                   17.587(4)
_cell_measurement_temperature    168(2)
_cell_volume                     8147(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  '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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52215
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       wedge
_exptl_crystal_F_000             4140
_exptl_crystal_size_max          0.96
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0437P)²+22.6098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                6782
_reflns_number_total             8326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            908430dsup1.cif
_cod_data_source_block           cvdd
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C30 H24 Cl5 Cu2.50 N9 O6 P3'
_cod_database_code               7027829
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_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
Cu1 Cu 0.092981(15) 0.159045(17) 0.57993(2) 0.02482(9) Uani 1 1 d .
Cu2 Cu 0.0000 0.34130(2) 0.2500 0.02236(11) Uani 1 2 d S
Cu3 Cu 0.230396(18) 0.330461(18) 0.99000(3) 0.03366(11) Uani 1 1 d .
Cl1 Cl 0.08891(3) 0.05811(4) 0.63202(5) 0.03290(17) Uani 1 1 d .
Cl2 Cl 0.02933(3) 0.27080(4) 0.17803(5) 0.03107(16) Uani 1 1 d .
Cl3 Cl 0.26766(5) 0.41639(5) 0.95172(8) 0.0598(3) Uani 1 1 d .
Cl4 Cl 0.15943(3) 0.38095(4) 1.01156(5) 0.03310(17) Uani 1 1 d .
Cl5 Cl 0.24738(4) 0.25091(4) 0.90794(5) 0.0411(2) Uani 1 1 d .
P1 P 0.06360(3) 0.30880(4) 0.55434(4) 0.02119(15) Uani 1 1 d .
P2 P 0.13038(3) 0.25472(4) 0.47434(4) 0.02356(16) Uani 1 1 d .
P3 P 0.10626(3) 0.38863(4) 0.46643(4) 0.02422(16) Uani 1 1 d .
O1 O 0.00061(8) 0.28330(9) 0.53994(12) 0.0242(4) Uani 1 1 d .
O2 O 0.08910(9) 0.32463(10) 0.65076(12) 0.0276(4) Uani 1 1 d .
O3 O 0.10446(9) 0.21283(10) 0.39158(12) 0.0275(4) Uani 1 1 d .
O4 O 0.19122(9) 0.21857(11) 0.52209(13) 0.0317(5) Uani 1 1 d .
O5 O 0.06877(9) 0.42846(10) 0.38379(12) 0.0281(4) Uani 1 1 d .
O6 O 0.15383(9) 0.44366(10) 0.51214(12) 0.0305(5) Uani 1 1 d .
N1 N 0.09589(10) 0.24788(11) 0.53253(14) 0.0219(5) Uani 1 1 d .
N2 N 0.13658(11) 0.32667(13) 0.44544(16) 0.0293(5) Uani 1 1 d .
N3 N 0.06252(10) 0.37599(12) 0.50882(14) 0.0252(5) Uani 1 1 d .
N16 N 0.00278(10) 0.16855(11) 0.51559(15) 0.0238(5) Uani 1 1 d .
N26 N 0.08345(11) 0.21865(13) 0.69900(15) 0.0290(5) Uani 1 1 d .
N36 N 0.10212(14) 0.11083(13) 0.45121(17) 0.0377(6) Uani 1 1 d .
N46 N 0.18360(11) 0.16651(13) 0.63642(15) 0.0283(5) Uani 1 1 d .
N56 N 0.05872(10) 0.41202(12) 0.25121(14) 0.0256(5) Uani 1 1 d .
N66 N 0.19419(11) 0.37764(13) 0.62877(16) 0.0325(6) Uani 1 1 d .
C11 C -0.02728(12) 0.22497(13) 0.50260(16) 0.0219(5) Uani 1 1 d .
C12 C -0.08685(12) 0.23055(15) 0.45894(18) 0.0264(6) Uani 1 1 d .
H12 H -0.1059 0.2722 0.4523 0.032 Uiso 1 1 calc R
C13 C -0.11768(13) 0.17317(16) 0.4253(2) 0.0344(7) Uani 1 1 d .
H13 H -0.1588 0.1743 0.3963 0.041 Uiso 1 1 calc R
C14 C -0.08739(14) 0.11361(16) 0.4346(2) 0.0379(8) Uani 1 1 d .
H14 H -0.1075 0.0739 0.4102 0.045 Uiso 1 1 calc R
C15 C -0.02834(14) 0.11311(15) 0.47931(19) 0.0315(7) Uani 1 1 d .
H15 H -0.0081 0.0723 0.4854 0.038 Uiso 1 1 calc R
C21 C 0.08469(12) 0.28342(15) 0.71110(18) 0.0272(6) Uani 1 1 d .
C22 C 0.08349(15) 0.31447(17) 0.7804(2) 0.0363(7) Uani 1 1 d .
H22 H 0.0849 0.3615 0.7855 0.044 Uiso 1 1 calc R
C23 C 0.08011(17) 0.27463(19) 0.8416(2) 0.0439(9) Uani 1 1 d .
H23 H 0.0791 0.2936 0.8905 0.053 Uiso 1 1 calc R
C24 C 0.07813(17) 0.20617(19) 0.8310(2) 0.0445(9) Uani 1 1 d .
H24 H 0.0758 0.1776 0.8725 0.053 Uiso 1 1 calc R
C25 C 0.07966(16) 0.18040(17) 0.7596(2) 0.0392(8) Uani 1 1 d .
H25 H 0.0780 0.1336 0.7526 0.047 Uiso 1 1 calc R
C31 C 0.09633(14) 0.14473(15) 0.38397(19) 0.0302(7) Uani 1 1 d .
C32 C 0.0826(2) 0.11874(19) 0.3060(2) 0.0495(10) Uani 1 1 d .
H32 H 0.0779 0.1462 0.2597 0.059 Uiso 1 1 calc R
C33 C 0.0759(3) 0.0507(2) 0.2983(3) 0.0739(15) Uani 1 1 d .
H33 H 0.0659 0.0300 0.2457 0.089 Uiso 1 1 calc R
C34 C 0.0838(3) 0.0131(2) 0.3670(3) 0.0820(18) Uani 1 1 d .
H34 H 0.0805 -0.0339 0.3630 0.098 Uiso 1 1 calc R
C35 C 0.0965(2) 0.04420(19) 0.4413(3) 0.0615(12) Uani 1 1 d .
H35 H 0.1016 0.0177 0.4885 0.074 Uiso 1 1 calc R
C41 C 0.21602(13) 0.19896(16) 0.60463(18) 0.0287(6) Uani 1 1 d .
C42 C 0.27471(14) 0.21253(18) 0.6477(2) 0.0381(8) Uani 1 1 d .
H42 H 0.2952 0.2375 0.6225 0.046 Uiso 1 1 calc R
C43 C 0.30252(15) 0.1890(2) 0.7275(2) 0.0439(9) Uani 1 1 d .
H43 H 0.3430 0.1961 0.7582 0.053 Uiso 1 1 calc R
C44 C 0.27020(15) 0.15453(19) 0.7625(2) 0.0409(8) Uani 1 1 d .
H44 H 0.2883 0.1379 0.8178 0.049 Uiso 1 1 calc R
C45 C 0.21184(14) 0.14492(17) 0.71610(19) 0.0349(7) Uani 1 1 d .
H45 H 0.1901 0.1220 0.7410 0.042 Uiso 1 1 calc R
C51 C 0.08780(12) 0.44391(14) 0.32205(18) 0.0266(6) Uani 1 1 d .
C52 C 0.13078(14) 0.49059(16) 0.3336(2) 0.0369(8) Uani 1 1 d .
H52 H 0.1506 0.5121 0.3857 0.044 Uiso 1 1 calc R
C53 C 0.14357(16) 0.50442(18) 0.2665(2) 0.0436(9) Uani 1 1 d .
H53 H 0.1730 0.5357 0.2716 0.052 Uiso 1 1 calc R
C54 C 0.11335(16) 0.47257(19) 0.1914(2) 0.0425(8) Uani 1 1 d .
H54 H 0.1216 0.4821 0.1444 0.051 Uiso 1 1 calc R
C55 C 0.07125(14) 0.42690(17) 0.1856(2) 0.0335(7) Uani 1 1 d .
H55 H 0.0504 0.4052 0.1339 0.040 Uiso 1 1 calc R
C61 C 0.19835(12) 0.43135(15) 0.58944(18) 0.0274(6) Uani 1 1 d .
C62 C 0.24208(15) 0.47858(17) 0.6180(2) 0.0458(9) Uani 1 1 d .
H62 H 0.2436 0.5152 0.5850 0.055 Uiso 1 1 calc R
C63 C 0.28336(19) 0.4685(2) 0.6983(3) 0.0732(16) Uani 1 1 d .
H63 H 0.3146 0.4989 0.7229 0.088 Uiso 1 1 calc R
C64 C 0.2786(2) 0.4134(2) 0.7426(3) 0.0728(15) Uani 1 1 d .
H64 H 0.3060 0.4068 0.7984 0.087 Uiso 1 1 calc R
C65 C 0.23476(16) 0.36872(19) 0.7062(2) 0.0443(9) Uani 1 1 d .
H65 H 0.2330 0.3304 0.7366 0.053 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'
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'
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'
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
N1 Cu1 N46 85.07(10) . .
N1 Cu1 N16 84.79(9) . .
N46 Cu1 N16 169.84(10) . .
N1 Cu1 Cl1 179.30(8) . .
N46 Cu1 Cl1 95.42(7) . .
N16 Cu1 Cl1 94.73(7) . .
N1 Cu1 N26 87.24(9) . .
N46 Cu1 N26 91.60(9) . .
N16 Cu1 N26 87.35(9) . .
Cl1 Cu1 N26 93.25(6) . .
N1 Cu1 N36 86.47(9) . .
N46 Cu1 N36 88.36(10) . .
N16 Cu1 N36 91.57(10) . .
Cl1 Cu1 N36 93.03(7) . .
N26 Cu1 N36 173.70(9) . .
N56 Cu2 N56 91.86(14) . 2
N56 Cu2 Cl2 92.47(7) . .
N56 Cu2 Cl2 147.84(7) 2 .
N56 Cu2 Cl2 147.84(7) . 2
N56 Cu2 Cl2 92.47(7) 2 2
Cl2 Cu2 Cl2 100.50(5) . 2
Cl3 Cu3 Cl4 99.58(4) . .
Cl3 Cu3 Cl5 98.22(4) . .
Cl4 Cu3 Cl5 142.38(4) . .
Cl3 Cu3 Cl5 142.41(5) . 7_557
Cl4 Cu3 Cl5 98.48(3) . 7_557
Cl5 Cu3 Cl5 86.88(4) . 7_557
Cu3 Cl5 Cu3 93.12(4) . 7_557
N3 P1 O2 106.76(12) . .
N3 P1 O1 113.00(12) . .
O2 P1 O1 100.25(11) . .
N3 P1 N1 116.30(13) . .
O2 P1 N1 112.80(12) . .
O1 P1 N1 106.66(11) . .
N2 P2 O3 104.76(13) . .
N2 P2 O4 113.10(13) . .
O3 P2 O4 100.85(12) . .
N2 P2 N1 116.18(13) . .
O3 P2 N1 114.68(12) . .
O4 P2 N1 106.38(12) . .
N2 P3 N3 118.58(13) . .
N2 P3 O6 109.36(13) . .
N3 P3 O6 113.61(13) . .
N2 P3 O5 110.35(13) . .
N3 P3 O5 104.09(12) . .
O6 P3 O5 98.86(11) . .
C11 O1 P1 128.98(18) . .
C21 O2 P1 125.12(18) . .
C31 O3 P2 127.51(19) . .
C41 O4 P2 127.51(19) . .
C51 O5 P3 124.15(19) . .
C61 O6 P3 120.81(19) . .
P2 N1 P1 123.37(15) . .
P2 N1 Cu1 118.00(13) . .
P1 N1 Cu1 118.63(13) . .
P2 N2 P3 122.15(16) . .
P1 N3 P3 120.62(16) . .
C11 N16 C15 116.1(2) . .
C11 N16 Cu1 125.90(19) . .
C15 N16 Cu1 117.89(19) . .
C21 N26 C25 116.2(3) . .
C21 N26 Cu1 127.11(19) . .
C25 N26 Cu1 116.6(2) . .
C31 N36 C35 115.5(3) . .
C31 N36 Cu1 125.4(2) . .
C35 N36 Cu1 116.6(2) . .
C41 N46 C45 115.9(3) . .
C41 N46 Cu1 125.0(2) . .
C45 N46 Cu1 118.5(2) . .
C51 N56 C55 117.6(3) . .
C51 N56 Cu2 117.8(2) . .
C55 N56 Cu2 124.5(2) . .
C61 N66 C65 117.1(3) . .
N16 C11 C12 125.2(3) . .
N16 C11 O1 119.9(2) . .
C12 C11 O1 114.7(2) . .
C11 C12 C13 117.5(3) . .
C12 C13 C14 118.9(3) . .
C15 C14 C13 119.2(3) . .
N16 C15 C14 123.0(3) . .
N26 C21 C22 125.6(3) . .
N26 C21 O2 118.2(3) . .
C22 C21 O2 116.2(3) . .
C23 C22 C21 117.3(3) . .
C22 C23 C24 119.0(3) . .
C25 C24 C23 119.0(3) . .
N26 C25 C24 122.9(3) . .
N36 C31 C32 126.0(3) . .
N36 C31 O3 117.9(3) . .
C32 C31 O3 116.1(3) . .
C31 C32 C33 116.5(4) . .
C34 C33 C32 119.6(4) . .
C35 C34 C33 119.0(4) . .
N36 C35 C34 123.3(4) . .
N46 C41 O4 119.2(3) . .
N46 C41 C42 124.6(3) . .
O4 C41 C42 116.1(3) . .
C43 C42 C41 118.4(3) . .
C42 C43 C44 118.6(3) . .
C45 C44 C43 119.1(3) . .
N46 C45 C44 123.4(3) . .
N56 C51 C52 124.4(3) . .
N56 C51 O5 113.0(2) . .
C52 C51 O5 122.5(3) . .
C53 C52 C51 117.2(3) . .
C52 C53 C54 119.7(3) . .
C55 C54 C53 119.2(3) . .
N56 C55 C54 121.9(3) . .
N66 C61 C62 126.8(3) . .
N66 C61 O6 117.2(3) . .
C62 C61 O6 116.0(3) . .
C63 C62 C61 115.1(4) . .
C62 C63 C64 119.2(4) . .
C65 C64 C63 120.3(3) . .
N66 C65 C64 121.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.988(2) .
Cu1 N46 2.090(3) .
Cu1 N16 2.093(2) .
Cu1 Cl1 2.2492(9) .
Cu1 N26 2.509(3) .
Cu1 N36 2.559(3) .
Cu2 N56 2.048(2) .
Cu2 N56 2.048(2) 2
Cu2 Cl2 2.2204(8) .
Cu2 Cl2 2.2204(8) 2
Cu3 Cl3 2.2019(11) .
Cu3 Cl4 2.2208(10) .
Cu3 Cl5 2.3104(9) .
Cu3 Cl5 2.3236(10) 7_557
Cl5 Cu3 2.3236(10) 7_557
P1 N3 1.567(2) .
P1 O2 1.581(2) .
P1 O1 1.587(2) .
P1 N1 1.603(2) .
P2 N2 1.565(3) .
P2 O3 1.575(2) .
P2 O4 1.592(2) .
P2 N1 1.597(2) .
P3 N2 1.584(3) .
P3 N3 1.584(3) .
P3 O6 1.589(2) .
P3 O5 1.589(2) .
O1 C11 1.389(3) .
O2 C21 1.387(4) .
O3 C31 1.385(4) .
O4 C41 1.383(4) .
O5 C51 1.390(4) .
O6 C61 1.386(3) .
N16 C11 1.333(4) .
N16 C15 1.364(4) .
N26 C21 1.320(4) .
N26 C25 1.350(4) .
N36 C31 1.321(4) .
N36 C35 1.353(5) .
N46 C41 1.335(4) .
N46 C45 1.358(4) .
N56 C51 1.325(4) .
N56 C55 1.349(4) .
N66 C61 1.311(4) .
N66 C65 1.339(4) .
C11 C12 1.383(4) .
C12 C13 1.383(4) .
C13 C14 1.395(5) .
C14 C15 1.370(5) .
C21 C22 1.381(4) .
C22 C23 1.373(5) .
C23 C24 1.390(5) .
C24 C25 1.374(5) .
C31 C32 1.374(5) .
C32 C33 1.381(5) .
C33 C34 1.370(6) .
C34 C35 1.363(6) .
C41 C42 1.386(4) .
C42 C43 1.372(5) .
C43 C44 1.391(5) .
C44 C45 1.373(5) .
C51 C52 1.385(4) .
C52 C53 1.373(5) .
C53 C54 1.383(5) .
C54 C55 1.376(5) .
C61 C62 1.385(4) .
C62 C63 1.384(5) .
C63 C64 1.388(7) .
C64 C65 1.365(6) .
