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#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/05/7050564.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_7050564
loop_
_publ_author_name
'Grosshans, Philippe'
'Jouaiti, Abdelaziz'
'Hosseini, Mir Wais'
'Kyritsakas, Nathalie'
_publ_section_title
;
 Gradual increase in the dimensionality of cobalt and mercury
 coordination networks based on conformation of tetradentate tectons
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              793
_journal_paper_doi               10.1039/b301351k
_journal_volume                  27
_journal_year                    2003
_chemical_formula_moiety         'C60 H64 Cl10 Co2 N8 O23'
_chemical_formula_sum            'C60 H64 Cl10 Co2 N8 O23'
_chemical_formula_weight         1737.61
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0678(9)
_cell_length_b                   13.0678(9)
_cell_length_c                   25.914(1)
_cell_measurement_reflns_used    9331
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     4425.3(5)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
9331 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  0.3 deg 1 scans of   90 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00  327 frames
Set 2 Theta =   -6.00 Kappa = -174.00 Phi   =    0.00  141 frames
Friedel pairs were averaged. Internal R = 0.08
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            9331
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.30
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.907
_refine_diff_density_min         -0.610
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.726
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    9
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2101
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.186
_refine_ls_R_factor_gt           0.143
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.323
_refine_ls_wR_factor_ref         0.173
_reflns_number_gt                2101
_reflns_number_total             5179
_reflns_threshold_expression     >3.0σ(I)
_cod_data_source_file            b301351k.txt
_cod_data_source_block           st1231
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7050564
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,+z
-y,1/2+x,1/2+z
1/2+y,-x,1/2+z
-x,-y,-z
1/2+x,1/2+y,-z
+y,1/2-x,1/2-z
1/2-y,+x,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
CO 0.2500 0.2500 0.6187(1) 0.027(1) 0.500 Uani ? ? Co
CL 0.3278(3) 0.0824(3) 0.6190(2) 0.040(2) 1.000 Uani ? ? Cl
N1 0.143(1) 0.200(1) 0.5590(4) 0.030(7) 1.000 Uani ? ? N
C1 0.171(1) 0.141(2) 0.5198(6) 0.04(1) 1.000 Uani ? ? C
C2 0.107(1) 0.115(1) 0.4779(6) 0.037(9) 1.000 Uani ? ? C
C3 0.006(1) 0.153(1) 0.4801(5) 0.028(8) 1.000 Uani ? ? C
C4 -0.025(1) 0.210(1) 0.5211(6) 0.040(9) 1.000 Uani ? ? C
C5 0.048(1) 0.232(1) 0.5595(6) 0.042(9) 1.000 Uani ? ? C
C6 -0.063(1) 0.131(1) 0.4349(5) 0.027(8) 1.000 Uani ? ? C
O1 -0.037(1) 0.080(1) 0.3989(5) 0.056(8) 1.000 Uani ? ? O
O2 -0.1541(8) 0.1745(8) 0.4421(4) 0.030(5) 1.000 Uani ? ? O
C7 -0.232(1) 0.154(1) 0.4028(6) 0.028(8) 1.000 Uani ? ? C
C8 -0.2500 0.2500 0.3694(8) 0.03(1) 0.500 Uani ? ? C
C9 -0.344(1) 0.232(1) 0.3362(5) 0.032(8) 1.000 Uani ? ? C
O3 -0.3171(9) 0.1491(9) 0.3023(4) 0.037(6) 1.000 Uani ? ? O
C10 -0.390(1) 0.115(2) 0.2691(7) 0.05(1) 1.000 Uani ? ? C
C11 -0.359(1) 0.031(1) 0.2365(5) 0.026(8) 1.000 Uani ? ? C
C12 0.490(1) 0.262(1) 0.7405(5) 0.027(8) 1.000 Uani ? ? C
C13 0.409(1) 0.235(1) 0.7090(5) 0.032(8) 1.000 Uani ? ? C
N2 0.367(1) 0.298(1) 0.6744(4) 0.029(7) 1.000 Uani ? ? N
C14 0.409(1) 0.392(1) 0.6704(5) 0.028(8) 1.000 Uani ? ? C
C15 0.490(1) 0.424(1) 0.7000(6) 0.035(9) 1.000 Uani ? ? C
O4 -0.474(1) 0.155(1) 0.2677(6) 0.11(1) 1.000 Uani ? ? O
O5 0.176(2) 0.173(2) 0.323(1) 0.13(2) 1.000 Uani ? ? O
C18 0.011(1) 0.074(1) 0.0769(6) 0.21(4) 0.500 Uiso ? ? C
CL1 -0.0880(1) 0.1827(1) 0.0948(6) 0.23(1) 0.500 Uiso ? ? Cl
CL2 -0.0031(1) 0.0662(1) 0.0032(6) 0.28(2) 0.500 Uiso ? ? Cl
CL3 0.1306(1) 0.1006(1) 0.0935(6) 0.121(6) 0.500 Uiso ? ? Cl
O6 -0.2500 0.2500 0.165(2) 0.06(1) 0.250 Uiso ? ? O
O7 -0.055(3) 0.115(3) 0.156(2) 0.12(1) 0.500 Uiso ? ? O
H1 0.2389 0.1147 0.5200 0.0588 1.000 Uiso calc C1 H
H2 0.1303 0.0750 0.4499 0.0510 1.000 Uiso calc C2 H
H3 -0.0935 0.2343 0.5238 0.0528 1.000 Uiso calc C4 H
H4 0.0272 0.2735 0.5878 0.0579 1.000 Uiso calc C5 H
H5 -0.2944 0.1358 0.4193 0.0394 1.000 Uiso calc C7 H
H6 -0.2100 0.0996 0.3814 0.0394 1.000 Uiso calc C7 H
H7 -0.3593 0.2919 0.3168 0.0453 1.000 Uiso calc C9 H
H8 -0.4007 0.2142 0.3570 0.0453 1.000 Uiso calc C9 H
H9 0.5180 0.2140 0.7644 0.0402 1.000 Uiso calc C12 H
H10 0.3808 0.1677 0.7122 0.0435 1.000 Uiso calc C13 H
H11 0.3819 0.4389 0.6459 0.0384 1.000 Uiso calc C14 H
H12 0.5171 0.4905 0.6956 0.0460 1.000 Uiso calc C15 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
Co ? 0.299 0.973 International_Tables_Vol_IV_Table_2.3.1
N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL CO N1 90.3(4) . . . ?
CL CO N2 87.9(4) . . . ?
N1 CO N2 175.7(5) . . . ?
C1 N1 C5 117(1) . . . ?
N1 C1 C2 123(1) . . . ?
C1 C2 C3 116(1) . . . ?
C2 C3 C4 119(1) . . . ?
C2 C3 C6 117(1) . . . ?
C4 C3 C6 122(1) . . . ?
C3 C4 C5 117(1) . . . ?
N1 C5 C4 124(1) . . . ?
C3 C6 O1 122(1) . . . ?
C3 C6 O2 109(1) . . . ?
O1 C6 O2 127(1) . . . ?
C6 O2 C7 116(1) . . . ?
O2 C7 C8 110(1) . . . ?
C7 C8 C7 111(1) . . 2_455 ?
C7 C8 C9 108.5(9) . . . ?
C7 C8 C9 108.8(9) . . 2_455 ?
C7 C8 C9 108.8(9) 2_455 . . ?
C7 C8 C9 108.5(9) 2_455 . 2_455 ?
C9 C8 C9 110(1) . . 2_455 ?
C8 C9 O3 105(1) . . . ?
C9 O3 C10 117(1) . . . ?
O3 C10 C11 114(1) . . . ?
O3 C10 O4 120(1) . . . ?
C11 C10 O4 124(1) . . . ?
C10 C11 C12 120(1) . . 3_544 ?
C10 C11 C15 121(1) . . 3_544 ?
C12 C11 C15 117(1) 3_544 . 3_544 ?
C11 C12 C13 119(1) 4_555 . . ?
C12 C13 N2 123(1) . . . ?
C13 N2 C14 116(1) . . . ?
N2 C14 C15 123(1) . . . ?
C11 C15 C14 120(1) 4_555 . . ?
CL1 C18 CL2 102.1(7) . . . ?
CL1 C18 CL3 114.0(8) . . . ?
CL2 C18 CL3 111.2(8) . . . ?
C18 CL1 O7 72(1) . . . ?
C18 CL2 CL2 98.3(4) . . 5_555 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
CO CL 2.415(4) . . ?
CO N1 2.19(1) . . ?
CO N2 2.19(1) . . ?
N1 C1 1.33(2) . . ?
N1 C5 1.30(2) . . ?
C1 C2 1.41(2) . . ?
C2 C3 1.41(2) . . ?
C3 C4 1.36(2) . . ?
C3 C6 1.50(2) . . ?
C4 C5 1.41(2) . . ?
C6 O1 1.20(2) . . ?
C6 O2 1.33(2) . . ?
O2 C7 1.47(2) . . ?
C7 C8 1.54(2) . . ?
C7 C8 1.54(2) . 2_455 ?
C8 C9 1.51(2) . . ?
C8 C9 1.51(2) . 2_455 ?
C9 O3 1.44(2) . . ?
O3 C10 1.36(2) . . ?
C10 C11 1.44(2) . . ?
C10 O4 1.21(2) . . ?
C11 C12 1.38(2) . 3_544 ?
C11 C15 1.38(2) . 3_544 ?
C12 C13 1.39(2) . . ?
C13 N2 1.34(2) . . ?
N2 C14 1.36(2) . . ?
C14 C15 1.36(2) . . ?
C18 CL1 1.98(2) . . ?
C18 CL2 1.92(1) . . ?
C18 CL3 1.66(2) . . ?
CL1 O7 1.86(4) . . ?
CL2 CL2 1.7409 . 5_555 ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
