#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/08/7210831.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_7210831
loop_
_publ_author_name
'Yang, Meng'
'OuYang, Zhen-Jie'
'Chen, Wen-Bin'
'Zhou, Rong-Fu'
'Li, Nan'
'Dong, Wen'
_publ_section_title
;
 Structures of six photochromic 3d complexes containing
 3,3′-azobis-1,2,4-triazole ligand
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              8529
_journal_paper_doi               10.1039/c3ce40736e
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C12 H34 Co N20 O6'
_chemical_formula_weight         613.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 98.479(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8920(3)
_cell_length_b                   7.2477(2)
_cell_length_c                   14.5382(4)
_cell_measurement_reflns_used    5784
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.530
_cell_measurement_theta_min      1.90
_cell_volume                     1239.35(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean none
_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_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9976
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             642.0
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.198
_refine_diff_density_max         0.779
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2848
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1208P)²+3.1866P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1980
_refine_ls_wR_factor_ref         0.2087
_reflns_number_gt                2279
_reflns_number_total             2858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40736e.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2/c
_cod_original_formula_sum        'C12 H34 Co N20 O6 '
_cod_database_code               7210831
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Co1 Co 0.5000 0.71401(10) 0.7500 0.0186(3) Uani 1 2 d SD
N1 N 0.6747(3) 0.7184(5) 0.7252(2) 0.0266(7) Uani 1 1 d .
N10 N 0.4596(3) 0.9019(5) 0.6408(2) 0.0279(7) Uani 1 1 d D
N9 N 0.4597(3) 0.5181(5) 0.6442(2) 0.0289(8) Uani 1 1 d D
N2 N 0.7680(3) 0.7450(5) 0.7861(2) 0.0272(8) Uani 1 1 d .
N3 N 0.8145(3) 0.6945(6) 0.6464(3) 0.0346(9) Uani 1 1 d .
C1 C 0.7021(3) 0.6868(6) 0.6422(3) 0.0265(9) Uani 1 1 d .
H1 H 0.6508 0.6627 0.5888 0.032 Uiso 1 1 calc R
C2 C 0.8521(3) 0.7292(6) 0.7350(3) 0.0247(8) Uani 1 1 d .
N4 N 0.9653(3) 0.7390(5) 0.7783(3) 0.0278(7) Uani 1 1 d .
C6 C 0.4459(4) 0.8010(7) 0.5516(3) 0.0331(10) Uani 1 1 d D
C5 C 0.3951(4) 0.6128(7) 0.5630(3) 0.0330(9) Uani 1 1 d D
N7 N 0.8065(3) 0.2242(5) 0.7987(3) 0.0324(8) Uani 1 1 d .
H7 H 0.8414 0.2375 0.8545 0.039 Uiso 1 1 calc R
C4 C 0.8518(4) 0.2040(6) 0.7220(3) 0.0294(9) Uani 1 1 d .
N5 N 0.6751(3) 0.1955(6) 0.6794(3) 0.0407(10) Uani 1 1 d .
N6 N 0.7732(3) 0.1873(6) 0.6472(3) 0.0372(9) Uani 1 1 d .
C3 C 0.6937(3) 0.2196(6) 0.7706(3) 0.0278(9) Uani 1 1 d .
H3 H 0.6380 0.2314 0.8088 0.033 Uiso 1 1 calc R
N8 N 0.9668(3) 0.2011(5) 0.7120(3) 0.0320(8) Uani 1 1 d .
O1 O 0.8526(3) 0.0977(5) 0.4758(2) 0.0384(8) Uani 1 1 d D
O2 O 0.9306(4) 0.2680(5) 0.9842(3) 0.0442(9) Uani 1 1 d D
H6 H 0.318(2) 0.617(9) 0.573(4) 0.053 Uiso 1 1 d D
H5 H 0.392(5) 0.542(7) 0.507(3) 0.053 Uiso 1 1 d D
H8 H 0.521(3) 0.794(8) 0.532(4) 0.053 Uiso 1 1 d D
H9 H 0.394(4) 0.868(8) 0.506(3) 0.053 Uiso 1 1 d D
H10 H 0.518(4) 0.985(7) 0.642(4) 0.053 Uiso 1 1 d D
H11 H 0.391(3) 0.955(8) 0.639(4) 0.053 Uiso 1 1 d D
H12 H 0.814(4) 0.111(10) 0.516(3) 0.066 Uiso 1 1 d D
H13 H 0.820(5) 0.126(10) 0.426(2) 0.066 Uiso 1 1 d D
O3 O 0.9602(5) 0.4578(7) 0.9614(3) 0.0753(14) Uani 1 1 d D
H15 H 0.959(8) 0.163(6) 0.975(5) 0.113 Uiso 1 1 d D
H14 H 0.904(8) 0.251(11) 1.034(4) 0.113 Uiso 1 1 d D
H16 H 0.992(6) 0.446(14) 0.911(4) 0.113 Uiso 1 1 d D
H17 H 0.899(5) 0.516(12) 0.936(5) 0.113 Uiso 1 1 d D
H2 H 0.482(4) 0.416(6) 0.680(3) 0.090 Uiso 1 1 d D
H4 H 0.522(2) 0.527(3) 0.619(2) 0.090 Uiso 1 1 d D
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'
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
N10 Co1 N10 98.8(2) 2_656 .
N10 Co1 N9 177.93(14) 2_656 .
N10 Co1 N9 83.22(14) . .
N10 Co1 N9 83.22(14) 2_656 2_656
N10 Co1 N9 177.93(14) . 2_656
N9 Co1 N9 94.7(2) . 2_656
N10 Co1 N1 89.01(13) 2_656 2_656
N10 Co1 N1 89.90(13) . 2_656
N9 Co1 N1 90.63(14) . 2_656
N9 Co1 N1 90.50(13) 2_656 2_656
N10 Co1 N1 89.90(13) 2_656 .
N10 Co1 N1 89.01(13) . .
N9 Co1 N1 90.50(13) . .
N9 Co1 N1 90.63(13) 2_656 .
N1 Co1 N1 178.3(2) 2_656 .
C1 N1 N2 109.9(3) . .
C1 N1 Co1 121.7(3) . .
N2 N1 Co1 128.4(3) . .
C6 N10 Co1 109.1(3) . .
C6 N10 H10 109(4) . .
Co1 N10 H10 109(4) . .
C6 N10 H11 102(4) . .
Co1 N10 H11 114(4) . .
H10 N10 H11 114(6) . .
C5 N9 Co1 107.9(3) . .
C5 N9 H2 154(4) . .
Co1 N9 H2 96(4) . .
C5 N9 H4 90(2) . .
Co1 N9 H4 98.1(17) . .
H2 N9 H4 96(2) . .
N1 N2 C2 103.7(3) . .
C2 N3 C1 104.2(3) . .
N1 C1 N3 109.5(3) . .
N1 C1 H1 125.3 . .
N3 C1 H1 125.3 . .
N3 C2 N2 112.6(4) . .
N3 C2 N4 127.7(4) . .
N2 C2 N4 119.6(4) . .
N4 N4 C2 112.8(5) 2_756 .
N10 C6 C5 110.2(3) . .
N10 C6 H8 107(4) . .
C5 C6 H8 113(3) . .
N10 C6 H9 109(4) . .
C5 C6 H9 108(4) . .
H8 C6 H9 110(5) . .
N9 C5 C6 109.8(3) . .
N9 C5 H6 107(4) . .
C6 C5 H6 113(4) . .
N9 C5 H5 112(4) . .
C6 C5 H5 111(4) . .
H6 C5 H5 103(5) . .
C4 N7 C3 104.7(4) . .
C4 N7 H7 127.6 . .
C3 N7 H7 127.6 . .
N7 C4 N6 112.1(4) . .
N7 C4 N8 128.3(4) . .
N6 C4 N8 119.6(4) . .
N6 N5 C3 109.6(4) . .
N5 N6 C4 104.9(4) . .
N5 C3 N7 108.7(4) . .
N5 C3 H3 125.7 . .
N7 C3 H3 125.7 . .
N8 N8 C4 114.0(5) 2_756 .
H12 O1 H13 112(4) . .
H15 O2 H14 102(3) . .
O3 O3 H16 111(6) 3_767 .
O3 O3 H17 121(6) 3_767 .
H16 O3 H17 97(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N10 2.093(4) 2_656
Co1 N10 2.093(4) .
Co1 N9 2.096(4) .
Co1 N9 2.096(4) 2_656
Co1 N1 2.160(3) 2_656
Co1 N1 2.160(3) .
N1 C1 1.315(5) .
N1 N2 1.328(5) .
N10 C6 1.477(6) .
N10 H10 0.91(2) .
N10 H11 0.90(2) .
N9 C5 1.478(6) .
N9 H2 0.924(16) .
N9 H4 0.87(2) .
N2 C2 1.336(5) .
N3 C2 1.323(5) .
N3 C1 1.331(5) .
C1 H1 0.9300 .
C2 N4 1.402(5) .
N4 N4 1.248(7) 2_756
C6 C5 1.510(7) .
C6 H8 0.97(2) .
C6 H9 0.96(2) .
C5 H6 0.95(2) .
C5 H5 0.96(2) .
N7 C4 1.316(6) .
N7 C3 1.344(5) .
N7 H7 0.8600 .
C4 N6 1.331(6) .
C4 N8 1.396(6) .
N5 N6 1.320(6) .
N5 C3 1.322(6) .
C3 H3 0.9300 .
N8 N8 1.260(7) 2_756
O1 H12 0.802(19) .
O1 H13 0.79(2) .
O2 H15 0.85(2) .
O2 H14 0.85(2) .
O3 O3 1.488(10) 3_767
O3 H16 0.88(2) .
O3 H17 0.88(2) .
