#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322378.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_4322378
loop_
_publ_author_name
'Ok-Sang Jung'
'Yong Tae Kim'
'Young-A Lee'
'Yun Ju Kim'
'Hee K. Chae'
_publ_section_title
;
 Trinucleating Bipyridyl Ligands; Synthesis and Structure of
 Cobalt-Benzoquinone Complex of Cyclotriphosphazenes Bearing
 Dioxybipyridine Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5457
_journal_page_last               5460
_journal_paper_doi               10.1021/ic990215d
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C38 H28 Cl2 N9 O6 P3'
_chemical_formula_weight         870.50
_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                 106.556(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.982(3)
_cell_length_b                   18.921(3)
_cell_length_c                   10.4381(15)
_cell_measurement_temperature    293(2)
_cell_volume                     4161.4(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.704
_diffrn_measured_fraction_theta_max 0.704
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2637
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.328
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          2.162
_refine_ls_shift/su_mean         0.162
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1526P)²+10.2816P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2145
_reflns_number_gt                2532
_reflns_number_total             2578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990215d.cif
_cod_data_source_block           C38H28Cl2N9O6P3
_cod_original_cell_volume        4161.5(10)
_cod_database_code               4322378
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
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.0000 0.17306(8) 0.2500 0.0351(5) Uani 1 2 d S . .
P2 P -0.06512(5) 0.29894(6) 0.20848(12) 0.0362(4) Uani 1 1 d . . .
O1 O -0.00391(15) 0.12090(16) 0.1296(3) 0.0404(8) Uani 1 1 d . . .
O2 O -0.10179(15) 0.33026(17) 0.0670(3) 0.0432(8) Uani 1 1 d . . .
O3 O -0.10978(16) 0.32067(17) 0.2973(3) 0.0438(8) Uani 1 1 d . . .
N1 N -0.06344(17) 0.2156(2) 0.2087(4) 0.0433(10) Uani 1 1 d . . .
N2 N 0.0000 0.3395(3) 0.2500 0.0462(14) Uani 1 2 d S . .
N3 N 0.0597(3) -0.0555(2) 0.2229(5) 0.0612(13) Uani 1 1 d . . .
N4 N -0.2664(2) 0.3840(3) 0.0105(6) 0.0658(14) Uani 1 1 d . . .
N5 N -0.1989(3) 0.4833(3) 0.1935(6) 0.0779(17) Uani 1 1 d . . .
C1 C 0.0364(2) 0.0617(2) 0.1456(5) 0.0390(11) Uani 1 1 d . . .
C2 C 0.0252(2) 0.0041(2) 0.2153(5) 0.0448(11) Uani 1 1 d . . .
C3 C 0.1052(3) -0.0544(3) 0.1624(7) 0.0705(18) Uani 1 1 d . . .
H3 H 0.1298 -0.0950 0.1689 0.085 Uiso 1 1 calc R . .
C4 C 0.1193(3) 0.0010(3) 0.0913(7) 0.0670(16) Uani 1 1 d . . .
H4 H 0.1521 -0.0018 0.0515 0.080 Uiso 1 1 calc R . .
C5 C 0.0828(3) 0.0613(3) 0.0810(6) 0.0550(14) Uani 1 1 d . . .
H5 H 0.0895 0.1002 0.0321 0.066 Uiso 1 1 calc R . .
C6 C -0.1678(2) 0.3309(2) 0.0138(5) 0.0415(11) Uani 1 1 d . . .
C7 C -0.2043(2) 0.3752(3) 0.0681(5) 0.0448(12) Uani 1 1 d . . .
C8 C -0.2917(3) 0.3473(4) -0.1028(8) 0.078(2) Uani 1 1 d . . .
H8 H -0.3346 0.3535 -0.1454 0.094 Uiso 1 1 calc R . .
C9 C -0.2587(3) 0.3015(4) -0.1597(7) 0.0699(18) Uani 1 1 d . . .
H9 H -0.2789 0.2768 -0.2371 0.084 Uiso 1 1 calc R . .
C10 C -0.1946(3) 0.2931(3) -0.0990(6) 0.0567(14) Uani 1 1 d . . .
H10 H -0.1704 0.2625 -0.1342 0.068 Uiso 1 1 calc R . .
C11 C -0.1299(2) 0.3908(3) 0.2977(6) 0.0478(12) Uani 1 1 d . . .
C12 C -0.1759(2) 0.4168(3) 0.1909(6) 0.0516(13) Uani 1 1 d . . .
C13 C -0.1751(5) 0.5208(4) 0.3010(9) 0.098(3) Uani 1 1 d . . .
H13 H -0.1905 0.5664 0.3036 0.118 Uiso 1 1 calc R . .
C14 C -0.1284(4) 0.4971(4) 0.4113(9) 0.096(3) Uani 1 1 d . . .
H14 H -0.1132 0.5262 0.4853 0.115 Uiso 1 1 calc R . .
C15 C -0.1049(3) 0.4305(4) 0.4102(7) 0.0677(16) Uani 1 1 d . . .
H15 H -0.0733 0.4129 0.4825 0.081 Uiso 1 1 calc R . .
C21 C 0.5000 0.0446(7) 0.2500 0.111(4) Uani 1 2 d S . .
H21A H 0.4843 0.0277 0.3213 0.166 Uiso 0.50 1 calc PR . .
H21B H 0.5425 0.0277 0.2625 0.166 Uiso 0.50 1 calc PR . .
H21C H 0.4732 0.0277 0.1661 0.166 Uiso 0.50 1 calc PR . .
C22 C 0.5000 0.1245(7) 0.2500 0.088(3) Uani 1 2 d S . .
C23 C 0.4769(5) 0.1630(5) 0.3398(9) 0.098(3) Uani 1 1 d . . .
H23 H 0.4600 0.1376 0.3979 0.118 Uiso 1 1 calc R . .
C24 C 0.4769(4) 0.2340(4) 0.3495(8) 0.076(2) Uani 1 1 d . . .
H24 H 0.4632 0.2568 0.4151 0.092 Uiso 1 1 calc R . .
C25 C 0.5000 0.2738(6) 0.2500 0.098(4) Uani 1 2 d S . .
H25 H 0.5000 0.3229 0.2500 0.117 Uiso 1 2 calc SR . .
C26 C 0.2452(10) 0.2056(13) -0.021(2) 0.114(6) Uiso 0.50 1 d P . .
Cl1 Cl 0.3033(6) 0.2420(6) 0.0482(13) 0.228(4) Uiso 0.50 1 d P . .
Cl2 Cl 0.2391(8) 0.1354(10) -0.0250(15) 0.301(7) Uiso 0.50 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
_geom_angle_publ_flag
O1 P1 O1 102.8(2) . 2 ?
O1 P1 N1 112.5(2) . 2 ?
O1 P1 N1 105.10(19) 2 2 ?
O1 P1 N1 105.10(19) . . ?
O1 P1 N1 112.5(2) 2 . ?
N1 P1 N1 117.9(3) 2 . ?
N1 P2 N2 117.9(2) . . ?
N1 P2 O2 112.4(2) . . ?
N2 P2 O2 104.85(17) . . ?
N1 P2 O3 106.1(2) . . ?
N2 P2 O3 112.29(17) . . ?
O2 P2 O3 102.29(18) . . ?
C1 O1 P1 120.8(3) . . ?
C6 O2 P2 124.7(3) . . ?
C11 O3 P2 119.8(3) . . ?
P2 N1 P1 122.3(2) . . ?
P2 N2 P2 121.6(3) . 2 ?
C3 N3 C2 116.6(5) . . ?
C8 N4 C7 116.4(6) . . ?
C13 N5 C12 117.4(6) . . ?
C2 C1 C5 121.8(5) . . ?
C2 C1 O1 119.6(4) . . ?
C5 C1 O1 118.4(4) . . ?
N3 C2 C1 120.8(5) . . ?
N3 C2 C2 117.2(4) . 2 ?
C1 C2 C2 122.0(3) . 2 ?
N3 C3 C4 125.9(5) . . ?
C3 C4 C5 117.3(6) . . ?
C1 C5 C4 117.5(5) . . ?
C10 C6 C7 120.9(5) . . ?
C10 C6 O2 118.9(5) . . ?
C7 C6 O2 119.9(5) . . ?
N4 C7 C6 121.7(5) . . ?
N4 C7 C12 116.6(5) . . ?
C6 C7 C12 121.7(5) . . ?
N4 C8 C9 124.7(6) . . ?
C10 C9 C8 118.1(6) . . ?
C9 C10 C6 118.1(6) . . ?
C15 C11 C12 121.6(5) . . ?
C15 C11 O3 118.3(5) . . ?
C12 C11 O3 120.0(5) . . ?
N5 C12 C11 120.7(6) . . ?
N5 C12 C7 116.2(5) . . ?
C11 C12 C7 123.1(4) . . ?
N5 C13 C14 124.1(6) . . ?
C15 C14 C13 119.2(7) . . ?
C11 C15 C14 117.0(7) . . ?
C23 C22 C23 116.9(12) 2_655 . ?
C23 C22 C21 121.5(6) 2_655 . ?
C23 C22 C21 121.5(6) . . ?
C24 C23 C22 125.4(9) . . ?
C23 C24 C25 116.5(7) . . ?
C24 C25 C24 119.1(10) 2_655 . ?
Cl2 C26 Cl1 123.7(19) . . ?
Cl2 C26 Cl1 129(2) . 7 ?
Cl1 C26 Cl1 105.7(18) . 7 ?
Cl2 C26 C26 167(2) . 7 ?
Cl1 C26 C26 52.2(12) . 7 ?
Cl1 C26 C26 53.5(13) 7 7 ?
C26 Cl1 C26 74.3(18) . 7 ?
C26 Cl1 Cl1 36.8(10) . 7 ?
C26 Cl1 Cl1 37.5(10) 7 7 ?
C26 Cl1 Cl2 26.9(10) . . ?
C26 Cl1 Cl2 100.3(14) 7 . ?
Cl1 Cl1 Cl2 63.1(7) 7 . ?
C26 Cl1 Cl2 98.2(13) . 7 ?
C26 Cl1 Cl2 24.8(11) 7 7 ?
Cl1 Cl1 Cl2 61.7(7) 7 7 ?
Cl2 Cl1 Cl2 124.8(7) . 7 ?
C26 Cl2 Cl1 29.4(11) . . ?
C26 Cl2 Cl1 26.6(11) . 7 ?
Cl1 Cl2 Cl1 55.2(7) . 7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1 1.581(3) . ?
P1 O1 1.581(3) 2 ?
P1 N1 1.561(4) 2 ?
P1 N1 1.561(4) . ?
P2 N1 1.578(4) . ?
P2 N2 1.572(3) . ?
P2 O2 1.582(4) . ?
P2 O3 1.584(3) . ?
O1 C1 1.408(5) . ?
O2 C6 1.399(6) . ?
O3 C11 1.399(6) . ?
N2 P2 1.572(3) 2 ?
N3 C3 1.326(8) . ?
N3 C2 1.348(7) . ?
N4 C8 1.347(10) . ?
N4 C7 1.335(7) . ?
N5 C13 1.305(10) . ?
N5 C12 1.359(7) . ?
C1 C2 1.371(7) . ?
C1 C5 1.376(7) . ?
C2 C2 1.486(10) 2 ?
C3 C4 1.372(9) . ?
C4 C5 1.380(8) . ?
C6 C10 1.360(8) . ?
C6 C7 1.387(7) . ?
C7 C12 1.482(8) . ?
C8 C9 1.368(11) . ?
C9 C10 1.379(9) . ?
C11 C15 1.370(8) . ?
C11 C12 1.367(8) . ?
C13 C14 1.380(12) . ?
C14 C15 1.362(10) . ?
C21 C22 1.513(17) . ?
C22 C23 1.392(10) 2_655 ?
C22 C23 1.392(10) . ?
C23 C24 1.346(10) . ?
C24 C25 1.485(9) . ?
C25 C24 1.485(9) 2_655 ?
C26 Cl2 1.33(3) . ?
C26 Cl1 1.45(2) . ?
C26 Cl1 1.42(2) 7 ?
C26 C26 1.74(5) 7 ?
Cl1 C26 1.42(2) 7 ?
Cl1 Cl1 2.29(3) 7 ?
Cl1 Cl2 2.45(2) . ?
Cl1 Cl2 2.48(2) 7 ?
Cl2 Cl1 2.48(2) 7 ?
