#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/06/4110628.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_4110628
loop_
_publ_author_name
'Vadapalli Chandrasekhar'
'Ramachandran Azhakar'
'Venkatasubbaiah Krishnan'
'Arunachalampillai Athimoolam'
'Balasubramanian Murugesa Pandian'
_publ_section_title
;
 Cyclocarbophosphazene-Containing Tetrameric Assemblies Formed by the
 Mediation of P-O-P and P-O-Cu Linkages
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6802
_journal_page_last               6803
_journal_paper_doi               10.1021/ja061635m
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C14.5 H17.5 Br Cu N8 O1.5 P'
_chemical_formula_weight         502.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           84
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c'
_symmetry_space_group_name_H-M   'P 42/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.930(3)
_cell_length_b                   19.930(3)
_cell_length_c                   14.509(4)
_cell_measurement_temperature    100(2)
_cell_volume                     5763(2)
_computing_cell_refinement       'Bruker SMART V5.628'
_computing_data_collection       'Bruker SMART V5.628'
_computing_data_reduction        'Bruker SAINT+ V6.45'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SAINT+ V6.45'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38544
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_type   'Bruker SADABS V2.10'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             2012
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .1
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         7474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0917P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1623
_reflns_number_gt                3730
_reflns_number_total             7474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061635msi20060417_074324_2.cif
_cod_data_source_block           compound4
_cod_original_cell_volume        5763(18)
_cod_original_formula_sum        'C14.50 H17.50 Br Cu N8 O1.50 P'
_cod_database_code               4110628
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z+1/2'
'y, -x, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z-1/2'
'-y, x, -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 0.72632(3) 0.38926(3) 0.5000 0.0523(2) Uani 1 2 d S
Cu2 Cu 0.34601(3) 0.05932(3) 0.5000 0.0477(2) Uani 1 2 d S
Br1 Br 0.82256(4) 0.29606(4) 0.5000 0.0791(2) Uani 1 2 d S
Br2 Br 0.77997(4) 0.49712(4) 0.5000 0.0835(3) Uani 1 2 d S
P1 P 0.51011(7) 0.27568(6) 0.5000 0.0401(3) Uani 1 2 d S
P2 P 0.49970(7) 0.12737(7) 0.5000 0.0445(3) Uani 1 2 d S
N1 N 0.54774(16) 0.30495(16) 0.59201(19) 0.0471(7) Uani 1 1 d .
N2 N 0.6394(2) 0.3428(2) 0.5000 0.0452(10) Uani 1 2 d S
N3 N 0.64393(16) 0.35566(16) 0.3452(2) 0.0508(8) Uani 1 1 d .
N4 N 0.70576(16) 0.38369(16) 0.3636(2) 0.0519(8) Uani 1 1 d .
N5 N 0.53019(16) 0.09074(16) 0.4087(2) 0.0523(8) Uani 1 1 d .
N6 N 0.4019(2) -0.0205(2) 0.5000 0.0439(10) Uani 1 2 d S
N7 N 0.39504(15) -0.01320(15) 0.6564(2) 0.0496(8) Uani 1 1 d .
N8 N 0.35017(16) 0.03826(16) 0.6377(2) 0.0522(8) Uani 1 1 d .
N9 N 0.2842(2) 0.1349(2) 0.5000 0.0498(11) Uani 1 2 d S
N10 N 0.3050(3) 0.1983(2) 0.5000 0.0521(12) Uani 1 2 d S
O1 O 0.43662(18) 0.28178(18) 0.5000 0.0486(9) Uani 1 2 d S
O2 O 0.53356(17) 0.19876(17) 0.5000 0.0506(9) Uani 1 2 d S
O3 O 0.42656(18) 0.13403(18) 0.5000 0.0543(10) Uani 1 2 d S
C1 C 0.60580(19) 0.33224(18) 0.5792(2) 0.0443(9) Uani 1 1 d .
C2 C 0.5710(3) 0.3241(3) 0.2096(3) 0.0928(18) Uani 1 1 d .
H2A H 0.5714 0.3327 0.1445 0.139 Uiso 1 1 calc R
H2B H 0.5318 0.3442 0.2365 0.139 Uiso 1 1 calc R
H2C H 0.5702 0.2766 0.2202 0.139 Uiso 1 1 calc R
C3 C 0.6319(2) 0.3532(2) 0.2521(3) 0.0597(11) Uani 1 1 d .
C4 C 0.6852(2) 0.3809(2) 0.2117(3) 0.0653(12) Uani 1 1 d .
H4 H 0.6912 0.3875 0.1488 0.078 Uiso 1 1 calc R
C5 C 0.7310(2) 0.3985(2) 0.2818(3) 0.0584(11) Uani 1 1 d .
C6 C 0.7990(3) 0.4298(3) 0.2730(4) 0.0840(15) Uani 1 1 d .
H6A H 0.7981 0.4743 0.2984 0.126 Uiso 1 1 calc R
H6B H 0.8114 0.4320 0.2091 0.126 Uiso 1 1 calc R
H6C H 0.8313 0.4031 0.3059 0.126 Uiso 1 1 calc R
C7 C 0.42560(19) -0.04486(18) 0.5791(3) 0.0440(9) Uani 1 1 d .
C8 C 0.4418(3) -0.0776(3) 0.7918(3) 0.0809(15) Uani 1 1 d .
H8A H 0.4258 -0.1211 0.7736 0.121 Uiso 1 1 calc R
H8B H 0.4390 -0.0734 0.8576 0.121 Uiso 1 1 calc R
H8C H 0.4876 -0.0725 0.7726 0.121 Uiso 1 1 calc R
C9 C 0.4001(2) -0.0249(2) 0.7477(3) 0.0619(11) Uani 1 1 d .
C10 C 0.3572(2) 0.0186(3) 0.7877(3) 0.0734(13) Uani 1 1 d .
H10 H 0.3483 0.0222 0.8504 0.088 Uiso 1 1 calc R
C11 C 0.3284(2) 0.0571(2) 0.7178(3) 0.0656(12) Uani 1 1 d .
C12 C 0.2770(3) 0.1112(3) 0.7273(4) 0.0876(16) Uani 1 1 d .
H12A H 0.2832 0.1438 0.6793 0.131 Uiso 1 1 calc R
H12B H 0.2818 0.1325 0.7862 0.131 Uiso 1 1 calc R
H12C H 0.2329 0.0920 0.7224 0.131 Uiso 1 1 calc R
C13 C 0.1752(4) 0.0750(4) 0.5000 0.098(3) Uani 1 2 d S
H13A H 0.1946 0.0421 0.4597 0.147 Uiso 0.50 1 calc PR
H13B H 0.1309 0.0860 0.4789 0.147 Uiso 0.50 1 calc PR
H13C H 0.1728 0.0571 0.5614 0.147 Uiso 0.50 1 calc PR
C14 C 0.2182(3) 0.1372(3) 0.5000 0.0672(17) Uani 1 2 d S
C15 C 0.1972(3) 0.2057(3) 0.5000 0.075(2) Uani 1 2 d S
H15 H 0.1534 0.2217 0.5000 0.091 Uiso 1 2 calc SR
C16 C 0.2532(3) 0.2421(3) 0.5000 0.0613(16) Uani 1 2 d S
C17 C 0.2638(4) 0.3160(3) 0.5000 0.088(2) Uani 1 2 d S
H17A H 0.2568 0.3333 0.4389 0.132 Uiso 0.50 1 calc PR
H17B H 0.3088 0.3258 0.5194 0.132 Uiso 0.50 1 calc PR
H17C H 0.2326 0.3367 0.5416 0.132 Uiso 0.50 1 calc PR
H51 H 0.344(3) 0.205(2) 0.5000 0.028(13) Uiso 1 2 d S
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N2 Cu1 N4 78.20(9) . .
N2 Cu1 N4 78.20(9) . 6_556
N4 Cu1 N4 155.78(18) . 6_556
N2 Cu1 Br2 144.55(13) . .
N4 Cu1 Br2 98.00(9) . .
N4 Cu1 Br2 98.00(9) 6_556 .
N2 Cu1 Br1 107.82(13) . .
N4 Cu1 Br1 96.16(9) . .
N4 Cu1 Br1 96.16(9) 6_556 .
Br2 Cu1 Br1 107.64(4) . .
N6 Cu2 N9 175.72(19) . .
N6 Cu2 N8 78.96(9) . 6_556
N9 Cu2 N8 100.64(9) . 6_556
N6 Cu2 N8 78.96(9) . .
N9 Cu2 N8 100.64(9) . .
N8 Cu2 N8 155.83(18) 6_556 .
N6 Cu2 O3 97.83(16) . .
N9 Cu2 O3 86.45(17) . .
N8 Cu2 O3 96.31(10) 6_556 .
N8 Cu2 O3 96.31(10) . .
O1 P1 O2 111.7(2) . .
O1 P1 N1 115.26(14) . .
O2 P1 N1 101.95(15) . .
O1 P1 N1 115.26(14) . 6_556
O2 P1 N1 101.95(15) . 6_556
N1 P1 N1 109.1(2) . 6_556
O3 P2 O2 110.2(2) . .
O3 P2 N5 114.33(14) . .
O2 P2 N5 104.18(15) . .
O3 P2 N5 114.33(14) . 6_556
O2 P2 N5 104.18(15) . 6_556
N5 P2 N5 108.7(2) . 6_556
C1 N1 P1 116.3(2) . .
C1 N2 C1 117.1(4) 6_556 .
C1 N2 Cu1 120.8(2) 6_556 .
C1 N2 Cu1 120.8(2) . .
C3 N3 N4 111.2(3) . .
C3 N3 C1 131.1(3) . 6_556
N4 N3 C1 117.6(3) . 6_556
C5 N4 N3 104.8(3) . .
C5 N4 Cu1 142.1(3) . .
N3 N4 Cu1 113.1(2) . .
C7 N5 P2 117.6(3) 5_656 .
C7 N6 C7 118.9(4) 6_556 .
C7 N6 Cu2 120.1(2) 6_556 .
C7 N6 Cu2 120.1(2) . .
C9 N7 N8 111.6(3) . .
C9 N7 C7 131.7(3) . .
N8 N7 C7 116.7(3) . .
C11 N8 N7 104.8(3) . .
C11 N8 Cu2 143.5(3) . .
N7 N8 Cu2 111.6(2) . .
C14 N9 N10 106.2(5) . .
C14 N9 Cu2 131.3(4) . .
N10 N9 Cu2 122.5(4) . .
N9 N10 C16 112.0(5) . .
P2 O2 P1 137.7(2) . .
P2 O3 Cu2 131.9(2) . .
N1 C1 N2 129.3(3) . .
N1 C1 N3 120.6(3) . 6_556
N2 C1 N3 110.0(3) . 6_556
C4 C3 N3 106.1(4) . .
C4 C3 C2 129.3(4) . .
N3 C3 C2 124.6(4) . .
C3 C4 C5 107.6(4) . .
N4 C5 C4 110.3(4) . .
N4 C5 C6 120.8(4) . .
C4 C5 C6 128.9(4) . .
N5 C7 N6 128.5(4) 5_656 .
N5 C7 N7 120.1(3) 5_656 .
N6 C7 N7 111.4(3) . .
C10 C9 N7 105.3(4) . .
C10 C9 C8 128.7(4) . .
N7 C9 C8 125.9(4) . .
C9 C10 C11 107.6(4) . .
N8 C11 C10 110.8(4) . .
N8 C11 C12 121.4(4) . .
C10 C11 C12 127.7(4) . .
N9 C14 C15 109.0(6) . .
N9 C14 C13 122.6(6) . .
C15 C14 C13 128.4(6) . .
C16 C15 C14 106.0(5) . .
C15 C16 N10 106.8(6) . .
C15 C16 C17 131.2(6) . .
N10 C16 C17 122.0(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.964(4) .
Cu1 N4 2.024(3) .
Cu1 N4 2.024(3) 6_556
Cu1 Br2 2.4010(11) .
Cu1 Br1 2.6700(12) .
Cu2 N6 1.941(4) .
Cu2 N9 1.946(4) .
Cu2 N8 2.044(3) 6_556
Cu2 N8 2.044(3) .
Cu2 O3 2.190(4) .
P1 O1 1.470(4) .
P1 O2 1.603(4) .
P1 N1 1.638(3) .
P1 N1 1.639(3) 6_556
P2 O3 1.464(4) .
P2 O2 1.575(4) .
P2 N5 1.630(3) .
P2 N5 1.630(3) 6_556
N1 C1 1.292(5) .
N2 C1 1.347(4) 6_556
N2 C1 1.347(4) .
N3 C3 1.374(5) .
N3 N4 1.379(4) .
N3 C1 1.413(4) 6_556
N4 C5 1.322(5) .
N5 C7 1.282(5) 5_656
N6 C7 1.333(4) 6_556
N6 C7 1.333(4) .
N7 C9 1.349(5) .
N7 N8 1.387(4) .
N7 C7 1.424(5) .
N8 C11 1.295(5) .
N9 C14 1.316(7) .
N9 N10 1.331(7) .
N10 C16 1.352(7) .
C1 N3 1.413(4) 6_556
C2 C3 1.479(6) .
C3 C4 1.334(6) .
C4 C5 1.409(6) .
C5 C6 1.499(6) .
C7 N5 1.282(5) 5_656
C8 C9 1.485(6) .
C9 C10 1.348(6) .
C10 C11 1.395(6) .
C11 C12 1.495(6) .
C13 C14 1.507(10) .
C14 C15 1.428(9) .
C15 C16 1.331(9) .
C16 C17 1.488(9) .
