#------------------------------------------------------------------------------
#$Date: 2015-08-08 04:59:42 +0300 (Sat, 08 Aug 2015) $
#$Revision: 153158 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/54/7035486.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_7035486
loop_
_publ_author_name
'Zhang, Xiu-Mei'
'Li, Peng'
'Gao, Wei'
'Liu, Jie-Ping'
'Gao, En-Qing'
_publ_section_title
;
 A new cube-based dodecanuclear cobalt(ii) cluster with azide and
 tetrazolate ligands exhibiting ferromagnetic ordering.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13581
_journal_page_last               13585
_journal_paper_doi               10.1039/c5dt02032h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C49 H84 Co12 N30 O31'
_chemical_formula_weight         2296.62
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-06-11 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   17.1591(15)
_cell_length_b                   17.1591(15)
_cell_length_c                   24.633(2)
_cell_measurement_reflns_used    4123
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.079
_cell_measurement_theta_min      2.835
_cell_volume                     6281.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SMART'
_computing_publication_material  'Bruker SMART'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.0821
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30817
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.013
_diffrn_reflns_theta_max         25.013
_diffrn_reflns_theta_min         2.741
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.603
_exptl_absorpt_correction_T_max  0.5811
_exptl_absorpt_correction_T_min  0.5324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bolck
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.380
_platon_squeeze_details
;
;
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2103
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1627P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2400
_refine_ls_wR_factor_ref         0.2678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1064
_reflns_number_total             2103
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02032h1.cif
_cod_data_source_block           t
_cod_depositor_comments          'Adding full bibliography for 7035486.cif.'
_cod_original_cell_volume        6281.2(12)
_cod_database_code               7035486
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.532
_shelx_estimated_absorpt_t_max   0.581
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.32518(9) 0.47858(9) 0.2500 0.0584(5) Uani 1 2 d S T P . .
Co2 Co 0.15918(5) 0.31837(11) 0.18647(7) 0.0846(7) Uani 1 2 d S T P . .
N1 N 0.4207(5) 0.4507(5) 0.1491(3) 0.0790(19) Uani 1 1 d . . . . .
N2 N 0.4224(4) 0.4997(4) 0.1904(2) 0.0711(18) Uani 1 1 d . . . . .
N3 N 0.2495(6) 0.3352(5) 0.2500 0.077(2) Uani 0.3333 2 d S T P A 2
N4 N 0.308(2) 0.3053(17) 0.2500 0.077(2) Uani 0.3333 2 d S T P A 2
N5 N 0.3515(19) 0.2650(17) 0.2500 0.077(2) Uani 0.3333 2 d S T P A 2
O1 O 0.3773(3) 0.6227(3) 0.2500 0.0422(18) Uani 1 4 d S T P A .
O2 O 0.2495(6) 0.3352(5) 0.2500 0.077(2) Uani 0.6667 2 d S T P A 1
O3 O 0.2303(2) 0.4606(4) 0.1911(2) 0.0576(16) Uani 1 2 d S T P A .
O4 O 0.0663(5) 0.3128(4) 0.1282(3) 0.113(2) Uani 1 1 d . . . . .
H4A H 0.0542 0.3542 0.1345 0.136 Uiso 1 1 d R U . . .
H4B H 0.0893 0.3202 0.0967 0.136 Uiso 1 1 d R U . . .
O5 O 0.0848(3) 0.1697(7) 0.1885(5) 0.154(4) Uani 1 2 d S T P A .
H5A H 0.0778 0.1555 0.2219 0.184 Uiso 1 2 d R U P . .
H5B H 0.0324 0.1454 0.1748 0.184 Uiso 0.5 1 d R U P . .
C1 C 0.4994(4) 0.5006(4) 0.1246(5) 0.091(4) Uani 1 2 d S T P . .
C2 C 0.5299(4) 0.4701(4) 0.0745(5) 0.093(4) Uani 1 2 d DS T P . .
C3 C 0.6109(7) 0.5268(8) 0.0511(5) 0.147(5) Uani 1 1 d D . . . .
H3 H 0.6477 0.5840 0.0653 0.177 Uiso 1 1 calc R U . . .
C4 C 0.6378(11) 0.4977(12) 0.0057(6) 0.169(6) Uani 1 1 d . . . . .
H4 H 0.6924 0.5363 -0.0109 0.203 Uiso 1 1 calc R U . . .
C5 C 0.5855(8) 0.4145(8) -0.0143(9) 0.160(8) Uani 1 2 d S T P . .
H5 H 0.6068 0.3932 -0.0419 0.192 Uiso 1 2 calc R U P . .
C6 C 0.2550(4) 0.5099(8) 0.1446(4) 0.069(3) Uani 1 2 d S T P . .
H6A H 0.2865 0.5729 0.1532 0.103 Uiso 1 2 d R U P A .
H6B H 0.2021 0.4951 0.1238 0.103 Uiso 1 1 d R U . . .
C7 C 0.3333 0.6667 0.2500 0.038(5) Uani 1 12 d S T P . .
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'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 '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
O3 Co1 O3 88.2(2) . 16_556
O3 Co1 N2 178.8(2) . 16_556
O3 Co1 N2 91.9(2) 16_556 16_556
O3 Co1 N2 91.9(2) . .
O3 Co1 N2 178.8(2) 16_556 .
N2 Co1 N2 88.0(3) 16_556 .
O3 Co1 N3 81.4(2) . .
O3 Co1 N3 81.4(2) 16_556 .
N2 Co1 N3 99.9(2) 16_556 .
N2 Co1 N3 99.9(2) . .
O3 Co1 O2 81.4(2) . .
O3 Co1 O2 81.4(2) 16_556 .
N2 Co1 O2 99.9(2) 16_556 .
N2 Co1 O2 99.9(2) . .
O3 Co1 O1 90.9(2) . .
O3 Co1 O1 90.9(2) 16_556 .
N2 Co1 O1 87.9(2) 16_556 .
N2 Co1 O1 87.9(2) . .
N3 Co1 O1 169.1(3) . .
O2 Co1 O1 169.1(3) . .
O3 Co1 Co1 45.04(11) . 20
O3 Co1 Co1 45.04(11) 16_556 20
N2 Co1 Co1 134.72(16) 16_556 20
N2 Co1 Co1 134.72(16) . 20
N3 Co1 Co1 88.2(2) . 20
O2 Co1 Co1 88.2(2) . 20
O1 Co1 Co1 80.95(16) . 20
O4 Co2 O4 94.1(4) 20 .
O4 Co2 O3 94.3(2) 20 .
O4 Co2 O3 94.3(2) . .
O4 Co2 O2 173.2(3) 20 20
O4 Co2 O2 91.2(3) . 20
O3 Co2 O2 80.9(2) . 20
O4 Co2 N3 173.2(3) 20 20
O4 Co2 N3 91.2(3) . 20
O3 Co2 N3 80.9(2) . 20
O4 Co2 N3 91.2(3) 20 .
O4 Co2 N3 173.2(3) . .
O3 Co2 N3 80.9(2) . .
N3 Co2 N3 83.1(4) 20 .
O4 Co2 O2 91.2(3) 20 .
O4 Co2 O2 173.2(3) . .
O3 Co2 O2 80.9(2) . .
O2 Co2 O2 83.1(4) 20 .
O4 Co2 O5 88.6(3) 20 .
O4 Co2 O5 88.6(3) . .
O3 Co2 O5 175.7(4) . .
O2 Co2 O5 95.8(3) 20 .
N3 Co2 O5 95.8(3) 20 .
N3 Co2 O5 95.8(3) . .
O2 Co2 O5 95.8(3) . .
N2 N1 C1 104.5(7) . .
N1 N2 N2 109.4(4) . 22_665
N1 N2 Co1 131.8(5) . .
N2 N2 Co1 118.74(17) 22_665 .
N4 N3 Co2 125.9(5) . .
N4 N3 Co2 125.9(5) . 16_556
Co2 N3 Co2 95.3(4) . 16_556
N4 N3 Co1 107.7(12) . .
Co2 N3 Co1 98.0(2) . .
Co2 N3 Co1 98.0(2) 16_556 .
N5 N4 N3 171(3) . .
C7 O1 Co1 129.05(16) . .
C7 O1 Co1 129.05(16) . 7_665
Co1 O1 Co1 101.9(3) . 7_665
Co2 O2 Co2 95.3(4) . 16_556
Co2 O2 Co1 98.0(2) . .
Co2 O2 Co1 98.0(2) 16_556 .
C6 O3 Co1 121.2(4) . 20
C6 O3 Co1 121.2(4) . .
Co1 O3 Co1 89.9(2) 20 .
C6 O3 Co2 119.5(6) . .
Co1 O3 Co2 99.5(2) 20 .
Co1 O3 Co2 99.5(2) . .
Co2 O4 H4A 109.3 . .
Co2 O4 H4B 109.3 . .
H4A O4 H4B 109.5 . .
Co2 O5 H5A 105.6 . .
Co2 O5 H5B 114.6 . .
H5A O5 H5B 106.2 . .
N1 C1 N1 112.3(10) . 22_665
N1 C1 C2 123.9(5) . .
N1 C1 C2 123.9(5) 22_665 .
C3 C2 C3 120.2(14) . 22_665
C3 C2 C1 119.8(7) . .
C3 C2 C1 119.8(7) 22_665 .
C2 C3 C4 119.0(13) . .
C2 C3 H3 120.5 . .
C4 C3 H3 120.5 . .
C5 C4 C3 120.7(17) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
C4 C5 C4 120(2) 22_665 .
C4 C5 H5 120.1 22_665 .
C4 C5 H5 120.1 . .
O3 C6 H6A 109.8 . .
O3 C6 H6B 109.1 . .
H6A C6 H6B 110.0 . .
O1 C7 O1 120.000(3) . 3_665
O1 C7 O1 120.000(1) . 14_566
O1 C7 O1 120.000(2) 3_665 14_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.086(4) .
Co1 O3 2.086(4) 16_556
Co1 N2 2.112(6) 16_556
Co1 N2 2.112(6) .
Co1 N3 2.132(7) .
Co1 O2 2.132(7) .
Co1 O1 2.168(5) .
Co1 Co1 2.947(3) 20
Co2 O4 2.111(7) 20
Co2 O4 2.111(7) .
Co2 O3 2.117(7) .
Co2 O2 2.118(6) 20
Co2 N3 2.118(6) 20
Co2 N3 2.118(6) .
Co2 O2 2.118(6) .
Co2 O5 2.210(10) .
N1 N2 1.312(7) .
N1 C1 1.329(8) .
N2 N2 1.337(13) 22_665
N3 N4 1.33(3) .
N3 Co2 2.118(6) 16_556
N4 N5 1.25(4) .
O1 C7 1.308(8) .
O1 Co1 2.168(5) 7_665
O2 Co2 2.118(6) 16_556
O3 C6 1.360(11) .
O3 Co1 2.085(4) 20
O4 H4A 0.8501 .
O4 H4B 0.8500 .
O5 H5A 0.8502 .
O5 H5B 0.8492 .
C1 N1 1.329(8) 22_665
C1 C2 1.532(16) .
C2 C3 1.363(8) .
C2 C3 1.363(8) 22_665
C3 C4 1.394(15) .
C3 H3 0.9300 .
C4 C5 1.343(16) .
C4 H4 0.9300 .
C5 C4 1.343(16) 22_665
C5 H5 0.9300 .
C6 H6A 0.9604 .
C6 H6B 0.9581 .
C7 O1 1.308(8) 3_665
C7 O1 1.308(8) 14_566
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O5 0.85 2.22 3.03(3) 160.2 16_556
O4 H4A N1 0.85 1.93 2.780(10) 178.5 20
O5 H5A O5 0.85 2.22 3.03(3) 160.2 16_556
O4 H4A N1 0.85 1.93 2.780(10) 178.5 20
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C1 N1 N2 N2 0.5(7) . 22_665
C1 N1 N2 Co1 177.0(7) . .
N2 N1 C1 N1 -0.8(13) . 22_665
N2 N1 C1 C2 178.2(10) . .
N1 C1 C2 C3 178.1(12) . .
N1 C1 C2 C3 -3.0(18) 22_665 .
N1 C1 C2 C3 3.0(18) . 22_665
N1 C1 C2 C3 -178.1(12) 22_665 22_665
C3 C2 C3 C4 -5(3) 22_665 .
C1 C2 C3 C4 179.7(13) . .
C2 C3 C4 C5 -1(3) . .
C3 C4 C5 C4 7(4) . 22_665
Co1 O1 C7 O1 180.0 . 3_665
Co1 O1 C7 O1 0.0 7_665 3_665
Co1 O1 C7 O1 0.0 . 14_566
Co1 O1 C7 O1 180.0 7_665 14_566
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.026 -0.019 -0.003 2254 383 ' '
2 0.000 0.000 0.250 7 0 ' '
3 0.000 0.000 0.750 7 0 ' '
4 0.087 0.174 0.750 8 2 ' '
5 0.087 0.913 0.750 8 2 ' '
6 0.174 0.087 0.250 8 2 ' '
7 0.826 0.913 0.750 9 2 ' '
8 0.913 0.087 0.250 8 2 ' '
9 0.913 0.826 0.250 9 2 ' '
