#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:01:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179499 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/96/4339675.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_4339675
loop_
_publ_author_name
'Ainscough, Eric W.'
'Brodie, Andrew M.'
'Derwahl, Andreas'
'Kirk, Steve'
'Otter, Carl A.'
_publ_section_title
;
 Conformationally rigid chelate rings in metal complexes of
 pyridyloxy-substituted 2,2'-dioxybiphenyl-cyclotetra- and
 cyclotriphosphazene platforms.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9841
_journal_page_last               9852
_journal_paper_doi               10.1021/ic701241v
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C48 H40 Cl4 Cu2 N8 O8 P4'
_chemical_formula_weight         1249.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.6564(3)
_cell_length_b                   23.6564(3)
_cell_length_c                   24.3070(7)
_cell_measurement_temperature    273(2)
_cell_volume                     13602.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            80874
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.800739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Acta Cryst., 1995, A51, 33'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5072
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.297
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6214
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0954P)²+39.5725P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1655
_reflns_number_gt                5289
_reflns_number_total             6214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701241v-file002.cif
_cod_data_source_block           c552
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               4339675
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.800562(18) 0.417804(18) 0.08693(2) 0.03818(17) Uani 1 1 d . . .
P2 P 0.97837(3) 0.57868(3) 0.03593(3) 0.0230(2) Uani 1 1 d D . .
P1 P 0.93879(3) 0.46299(3) 0.04322(3) 0.0252(2) Uani 1 1 d . . .
Cl2 Cl 0.79724(4) 0.32846(4) 0.11312(4) 0.0390(2) Uani 1 1 d . . .
Cl1 Cl 0.74128(4) 0.48941(4) 0.07766(5) 0.0558(3) Uani 1 1 d . . .
O4 O 0.92288(9) 0.61000(8) 0.01636(9) 0.0261(5) Uani 1 1 d . A .
O1 O 0.92165(9) 0.42703(9) 0.09645(10) 0.0295(5) Uani 1 1 d . A .
O2 O 0.87873(9) 0.47269(9) 0.01306(10) 0.0314(5) Uani 1 1 d . A .
N1 N 0.95906(12) 0.52186(11) 0.06311(12) 0.0304(6) Uani 1 1 d . A .
N2 N 1.02499(11) 0.57916(11) -0.00939(11) 0.0270(6) Uani 1 1 d . . .
C11 C 0.90080(14) 0.45056(13) 0.14464(15) 0.0315(7) Uani 1 1 d . . .
C41 C 0.92622(12) 0.66738(12) 0.00088(14) 0.0263(7) Uani 1 1 d . . .
C46 C 0.92981(16) 0.70819(15) 0.04135(16) 0.0384(8) Uani 1 1 d D A .
C42 C 0.92225(13) 0.67964(14) -0.05404(15) 0.0309(7) Uani 1 1 d . A .
H42 H 0.9207 0.6509 -0.0801 0.037 Uiso 1 1 calc R . .
C12 C 0.93707(16) 0.46961(15) 0.18438(16) 0.0377(8) Uani 1 1 d . A .
H12 H 0.9758 0.4709 0.1781 0.045 Uiso 1 1 calc R . .
N11 N 0.84502(13) 0.44817(13) 0.14997(14) 0.0383(7) Uani 1 1 d . A .
N21 N 0.81366(13) 0.40185(14) 0.00687(14) 0.0430(8) Uani 1 1 d . A .
C43 C 0.92067(15) 0.73601(15) -0.06996(18) 0.0400(9) Uani 1 1 d . . .
H43 H 0.9175 0.7453 -0.1070 0.048 Uiso 1 1 calc R A .
C23 C 0.84047(17) 0.38347(16) -0.10343(17) 0.0431(9) Uani 1 1 d . . .
C22 C 0.86830(15) 0.42417(15) -0.07301(16) 0.0361(8) Uani 1 1 d . A .
H22 H 0.8965 0.4462 -0.0889 0.043 Uiso 1 1 calc R . .
C21 C 0.85348(14) 0.43147(14) -0.01863(16) 0.0340(8) Uani 1 1 d . . .
C44 C 0.92376(15) 0.77795(14) -0.03136(19) 0.0439(10) Uani 1 1 d . A .
H44 H 0.9226 0.8156 -0.0424 0.053 Uiso 1 1 calc R . .
C45 C 0.92848(18) 0.76508(15) 0.0232(2) 0.0495(11) Uani 1 1 d . . .
H45 H 0.9309 0.7941 0.0489 0.059 Uiso 1 1 calc R A .
C26 C 0.8554(2) 0.37407(19) -0.16269(18) 0.0525(11) Uani 1 1 d . . .
H26A H 0.8487 0.4082 -0.1831 0.063 Uiso 1 1 calc R . .
H26B H 0.8324 0.3442 -0.1774 0.063 Uiso 1 1 calc R . .
H26C H 0.8946 0.3638 -0.1655 0.063 Uiso 1 1 calc R . .
C15 C 0.82347(17) 0.46599(19) 0.19830(19) 0.0501(11) Uani 1 1 d . . .
H15 H 0.7844 0.4658 0.2029 0.060 Uiso 1 1 calc R A .
C14 C 0.85640(19) 0.48420(19) 0.24050(18) 0.0522(11) Uani 1 1 d . A .
H14 H 0.8399 0.4949 0.2736 0.063 Uiso 1 1 calc R . .
C24 C 0.7987(2) 0.3523(2) -0.0771(2) 0.0550(11) Uani 1 1 d . A .
H24 H 0.7789 0.3247 -0.0964 0.066 Uiso 1 1 calc R . .
C13 C 0.91463(18) 0.48691(19) 0.23417(17) 0.0478(10) Uani 1 1 d . . .
C25 C 0.78686(19) 0.3620(2) -0.0228(2) 0.0561(11) Uani 1 1 d . . .
H25 H 0.7592 0.3402 -0.0058 0.067 Uiso 1 1 calc R A .
C16 C 0.9524(2) 0.5069(3) 0.2806(2) 0.0726(15) Uani 1 1 d . A .
H16A H 0.9619 0.4754 0.3038 0.087 Uiso 1 1 calc R . .
H16B H 0.9328 0.5349 0.3019 0.087 Uiso 1 1 calc R . .
H16C H 0.9863 0.5230 0.2657 0.087 Uiso 1 1 calc R . .
C31A C 0.9731(5) 0.6509(5) 0.1183(5) 0.044(2) Uani 0.606(10) 1 d PD A 1
C32A C 0.9809(5) 0.6395(5) 0.1736(5) 0.061(3) Uani 0.606(10) 1 d PD A 1
H32A H 1.0025 0.6087 0.1848 0.073 Uiso 0.606(10) 1 calc PR A 1
C33A C 0.9558(6) 0.6753(5) 0.2123(4) 0.080(4) Uani 0.606(10) 1 d PD A 1
H33A H 0.9605 0.6684 0.2497 0.096 Uiso 0.606(10) 1 calc PR A 1
C34A C 0.9239(6) 0.7210(5) 0.1950(4) 0.085(4) Uani 0.606(10) 1 d PD A 1
H34A H 0.9066 0.7442 0.2208 0.102 Uiso 0.606(10) 1 calc PR A 1
C35A C 0.9178(5) 0.7324(4) 0.1392(4) 0.066(3) Uani 0.606(10) 1 d PD A 1
H35A H 0.8977 0.7642 0.1280 0.079 Uiso 0.606(10) 1 calc PR A 1
C36A C 0.9414(5) 0.6967(5) 0.0998(3) 0.043(3) Uani 0.606(10) 1 d PD A 1
O3A O 1.0053(6) 0.6174(17) 0.0827(14) 0.029(3) Uani 0.606(10) 1 d PD A 1
C31B C 0.9613(8) 0.6459(8) 0.1195(7) 0.044(2) Uani 0.394(10) 1 d PD A 2
C32B C 0.9620(8) 0.6280(7) 0.1735(8) 0.061(3) Uani 0.394(10) 1 d PD A 2
H32B H 0.9855 0.5985 0.1842 0.073 Uiso 0.394(10) 1 calc PR A 2
C33B C 0.9268(8) 0.6548(7) 0.2120(6) 0.080(4) Uani 0.394(10) 1 d PD A 2
H33B H 0.9269 0.6435 0.2486 0.096 Uiso 0.394(10) 1 calc PR A 2
C34B C 0.8920(9) 0.6983(8) 0.1945(6) 0.085(4) Uani 0.394(10) 1 d PD A 2
H34B H 0.8683 0.7162 0.2197 0.102 Uiso 0.394(10) 1 calc PR A 2
C35B C 0.8921(8) 0.7154(7) 0.1401(6) 0.066(3) Uani 0.394(10) 1 d PD A 2
H35B H 0.8694 0.7457 0.1297 0.079 Uiso 0.394(10) 1 calc PR A 2
C36B C 0.9252(9) 0.6883(9) 0.1002(5) 0.043(3) Uani 0.394(10) 1 d PD A 2
O3B O 0.9991(10) 0.622(3) 0.082(2) 0.029(3) Uani 0.394(10) 1 d PD A 2
O9B O 0.7618(11) 0.6117(8) 0.1854(10) 0.112(10) Uani 0.232(11) 1 d P B 3
O9A O 0.8224(8) 0.6081(9) 0.1481(9) 0.045(8) Uani 0.132(10) 1 d P C 5
O9C O 0.7176(8) 0.6018(9) 0.1474(8) 0.043(7) Uani 0.137(10) 1 d P D 4
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
N11 Cu1 N21 137.07(12) . .
N11 Cu1 Cl2 98.17(9) . .
N21 Cu1 Cl2 96.03(10) . .
N11 Cu1 Cl1 97.87(10) . .
N21 Cu1 Cl1 98.24(11) . .
Cl2 Cu1 Cl1 137.74(4) . .
N2 P2 N1 120.71(14) . .
N2 P2 O4 111.81(14) . .
N1 P2 O4 106.68(13) . .
N2 P2 O3A 102.5(9) . .
N1 P2 O3A 108.0(19) . .
O4 P2 O3A 106.1(12) . .
N2 P2 O3B 105.6(15) . .
N1 P2 O3B 111(3) . .
O4 P2 O3B 99(2) . .
O3A P2 O3B 7(3) . .
N1 P1 N2 124.91(15) . 9_765
N1 P1 O1 107.68(14) . .
N2 P1 O1 103.12(13) 9_765 .
N1 P1 O2 106.61(14) . .
N2 P1 O2 109.68(14) 9_765 .
O1 P1 O2 102.68(12) . .
C41 O4 P2 119.00(18) . .
C11 O1 P1 124.0(2) . .
C21 O2 P1 122.3(2) . .
P1 N1 P2 136.9(2) . .
P1 N2 P2 139.56(18) 9_765 .
N11 C11 C12 124.7(3) . .
N11 C11 O1 114.8(3) . .
C12 C11 O1 120.3(3) . .
C42 C41 C46 123.4(3) . .
C42 C41 O4 117.4(3) . .
C46 C41 O4 119.1(3) . .
C41 C46 C45 116.2(4) . .
C41 C46 C36A 124.7(6) . .
C45 C46 C36A 118.7(6) . .
C41 C46 C36B 117.0(9) . .
C45 C46 C36B 126.1(9) . .
C36A C46 C36B 16.5(11) . .
C41 C42 C43 118.5(3) . .
C41 C42 H42 120.8 . .
C43 C42 H42 120.8 . .
C11 C12 C13 118.3(3) . .
C11 C12 H12 120.8 . .
C13 C12 H12 120.8 . .
C11 N11 C15 116.6(4) . .
C11 N11 Cu1 117.7(3) . .
C15 N11 Cu1 125.7(3) . .
C21 N21 C25 117.0(4) . .
C21 N21 Cu1 117.6(3) . .
C25 N21 Cu1 125.4(3) . .
C44 C43 C42 120.3(4) . .
C44 C43 H43 119.9 . .
C42 C43 H43 119.9 . .
C22 C23 C24 117.6(4) . .
C22 C23 C26 120.4(4) . .
C24 C23 C26 122.1(4) . .
C21 C22 C23 118.7(3) . .
C21 C22 H22 120.7 . .
C23 C22 H22 120.7 . .
N21 C21 C22 124.2(4) . .
N21 C21 O2 114.8(3) . .
C22 C21 O2 120.9(3) . .
C45 C44 C43 120.6(3) . .
C45 C44 H44 119.7 . .
C43 C44 H44 119.7 . .
C44 C45 C46 121.0(4) . .
C44 C45 H45 119.5 . .
C46 C45 H45 119.5 . .
C23 C26 H26A 109.5 . .
C23 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C23 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
N11 C15 C14 122.7(4) . .
N11 C15 H15 118.6 . .
C14 C15 H15 118.6 . .
C15 C14 C13 120.0(4) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C25 C24 C23 120.1(4) . .
C25 C24 H24 120.0 . .
C23 C24 H24 120.0 . .
C12 C13 C14 117.7(4) . .
C12 C13 C16 121.2(4) . .
C14 C13 C16 121.1(4) . .
N21 C25 C24 122.5(4) . .
N21 C25 H25 118.7 . .
C24 C25 H25 118.7 . .
C13 C16 H16A 109.5 . .
C13 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C13 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C32A C31A C36A 122.4(7) . .
C32A C31A O3A 115(2) . .
C36A C31A O3A 122(2) . .
C31A C32A C33A 118.7(7) . .
C31A C32A H32A 120.7 . .
C33A C32A H32A 120.7 . .
C34A C33A C32A 120.0(7) . .
C34A C33A H33A 120.0 . .
C32A C33A H33A 120.0 . .
C33A C34A C35A 120.3(7) . .
C33A C34A H34A 119.8 . .
C35A C34A H34A 119.8 . .
C34A C35A C36A 120.7(7) . .
C34A C35A H35A 119.7 . .
C36A C35A H35A 119.7 . .
C31A C36A C35A 117.8(7) . .
C31A C36A C46 123.7(9) . .
C35A C36A C46 118.4(8) . .
C31A O3A P2 123.2(11) . .
C32B C31B C36B 123.1(10) . .
C32B C31B O3B 120(4) . .
C36B C31B O3B 117(4) . .
C31B C32B C33B 119.3(10) . .
C31B C32B H32B 120.3 . .
C33B C32B H32B 120.3 . .
C34B C33B C32B 118.9(10) . .
C34B C33B H33B 120.5 . .
C32B C33B H33B 120.5 . .
C35B C34B C33B 120.6(10) . .
C35B C34B H34B 119.7 . .
C33B C34B H34B 119.7 . .
C34B C35B C36B 121.9(10) . .
C34B C35B H35B 119.0 . .
C36B C35B H35B 119.0 . .
C31B C36B C35B 116.0(9) . .
C31B C36B C46 119.8(14) . .
C35B C36B C46 123.6(13) . .
C31B O3B P2 121.2(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N11 1.993(3) .
Cu1 N21 2.006(4) .
Cu1 Cl2 2.2089(10) .
Cu1 Cl1 2.2108(11) .
P2 N2 1.559(3) .
P2 N1 1.566(3) .
P2 O4 1.581(2) .
P2 O3A 1.592(9) .
P2 O3B 1.594(12) .
P1 N1 1.550(3) .
P1 N2 1.551(3) 9_765
P1 O1 1.601(2) .
P1 O2 1.615(2) .
O4 C41 1.411(4) .
O1 C11 1.388(4) .
O2 C21 1.379(4) .
N2 P1 1.551(3) 9_765
C11 N11 1.327(4) .
C11 C12 1.368(6) .
C41 C42 1.369(5) .
C41 C46 1.381(5) .
C46 C45 1.416(5) .
C46 C36A 1.472(9) .
C46 C36B 1.510(12) .
C42 C43 1.389(5) .
C42 H42 0.9300 .
C12 C13 1.384(6) .
C12 H12 0.9300 .
N11 C15 1.348(5) .
N21 C21 1.328(5) .
N21 C25 1.346(6) .
C43 C44 1.367(6) .
C43 H43 0.9300 .
C23 C22 1.381(6) .
C23 C24 1.389(6) .
C23 C26 1.500(6) .
C22 C21 1.378(6) .
C22 H22 0.9300 .
C44 C45 1.366(7) .
C44 H44 0.9300 .
C45 H45 0.9300 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
C15 C14 1.358(7) .
C15 H15 0.9300 .
C14 C13 1.388(6) .
C14 H14 0.9300 .
C24 C25 1.369(7) .
C24 H24 0.9300 .
C13 C16 1.516(7) .
C25 H25 0.9300 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C31A C32A 1.383(9) .
C31A C36A 1.393(9) .
C31A O3A 1.400(10) .
C32A C33A 1.399(10) .
C32A H32A 0.9300 .
C33A C34A 1.383(11) .
C33A H33A 0.9300 .
C34A C35A 1.392(11) .
C34A H34A 0.9300 .
C35A C36A 1.393(9) .
C35A H35A 0.9300 .
C31B C32B 1.379(13) .
C31B C36B 1.399(12) .
C31B O3B 1.400(14) .
C32B C33B 1.403(13) .
C32B H32B 0.9300 .
C33B C34B 1.385(14) .
C33B H33B 0.9300 .
C34B C35B 1.384(14) .
C34B H34B 0.9300 .
C35B C36B 1.401(13) .
C35B H35B 0.9300 .
