#------------------------------------------------------------------------------
#$Date: 2019-05-01 05:01:09 +0300 (Wed, 01 May 2019) $
#$Revision: 214881 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/26/7232698.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_7232698
loop_
_publ_author_name
'Yang, Lili'
'Zhou, Jian'
'Zou, Hua-Hong'
'Tang, Qiuling'
_publ_section_title
;
 Three new metal coordination polymers of bifunctional
 imidazolate/tetrazolate bridges: the only example of a three-dimensional
 framework based on rare [Co4(μ3-OH)2(μ2-Cl)2]4+ mixed
 oxo-chloro-clusters
;
_journal_issue                   23
_journal_name_full               'RSC Advances'
_journal_page_first              13082
_journal_paper_doi               10.1039/C9RA01327J
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C20 H18 N12 Ni O2'
_chemical_formula_sum            'C20 H18 N12 Ni O2'
_chemical_formula_weight         517.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-01-22 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                102.237(3)
_cell_angle_beta                 98.119(4)
_cell_angle_gamma                106.700(3)
_cell_formula_units_Z            1
_cell_length_a                   7.4760(8)
_cell_length_b                   7.9402(7)
_cell_length_c                   9.3241(10)
_cell_measurement_reflns_used    4031
_cell_measurement_temperature    289(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      3.09
_cell_volume                     505.87(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      289(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4031
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.8984
_exptl_absorpt_correction_T_min  0.8732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             266
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         1755
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0534P)²+1.6505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1468
_reflns_number_gt                1292
_reflns_number_total             1755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ra01327j2.cif
_cod_data_source_block           1_CCDC1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7232698
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 1.0000 1.0000 1.0000 0.0284(4) Uani 1 2 d S
O1W O 0.8149(5) 0.7696(4) 1.0810(4) 0.0203(8) Uani 1 1 d D
N1 N 0.9371(6) 0.8343(5) 0.7653(4) 0.0171(9) Uani 1 1 d .
N2 N 0.8081(6) 0.6137(5) 0.5568(4) 0.0138(9) Uani 1 1 d .
N3 N 0.2346(6) -0.1234(5) 0.0671(5) 0.0165(9) Uani 1 1 d .
N4 N 0.1720(6) -0.3057(5) 0.0048(5) 0.0191(10) Uani 1 1 d .
N5 N 0.2960(6) -0.3746(5) 0.0586(5) 0.0195(10) Uani 1 1 d .
N6 N 0.4464(6) -0.2410(5) 0.1564(4) 0.0185(9) Uani 1 1 d .
C1 C 0.8776(7) 0.6572(6) 0.7055(5) 0.0165(11) Uani 1 1 d .
H1A H 0.8830 0.5723 0.7596 0.020 Uiso 1 1 calc R
C2 C 0.9032(7) 0.9088(6) 0.6478(5) 0.0188(11) Uani 1 1 d .
H2A H 0.9303 1.0329 0.6568 0.023 Uiso 1 1 calc R
C3 C 0.8255(8) 0.7771(6) 0.5187(6) 0.0222(12) Uani 1 1 d .
H3A H 0.7906 0.7920 0.4236 0.027 Uiso 1 1 calc R
C4 C 0.7151(7) 0.4364(6) 0.4539(5) 0.0147(10) Uani 1 1 d .
C5 C 0.6058(7) 0.4193(6) 0.3168(6) 0.0220(12) Uani 1 1 d .
H5A H 0.5963 0.5230 0.2895 0.026 Uiso 1 1 calc R
C6 C 0.5100(7) 0.2490(6) 0.2193(6) 0.0197(11) Uani 1 1 d .
H6A H 0.4375 0.2389 0.1263 0.024 Uiso 1 1 calc R
C7 C 0.5209(7) 0.0931(6) 0.2589(5) 0.0160(10) Uani 1 1 d .
C8 C 0.6350(7) 0.1120(7) 0.3968(6) 0.0236(12) Uani 1 1 d .
H8A H 0.6452 0.0083 0.4237 0.028 Uiso 1 1 calc R
C9 C 0.7329(8) 0.2813(6) 0.4943(6) 0.0228(12) Uani 1 1 d .
H9A H 0.8098 0.2922 0.5856 0.027 Uiso 1 1 calc R
C10 C 0.4027(7) -0.0884(6) 0.1599(5) 0.0137(10) Uani 1 1 d .
H1WB H 0.814(10) 0.661(4) 1.047(7) 0.06(2) Uiso 1 1 d D
H1WA H 0.719(6) 0.766(8) 1.121(6) 0.040(19) 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'
Ni Ni 0.3393 1.1124 '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'
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
N1 Ni1 N1 180.000(1) 2_777 .
N1 Ni1 O1W 85.69(14) 2_777 .
N1 Ni1 O1W 94.31(14) . .
N1 Ni1 O1W 94.31(14) 2_777 2_777
N1 Ni1 O1W 85.69(14) . 2_777
O1W Ni1 O1W 180.000(1) . 2_777
N1 Ni1 N3 90.79(14) 2_777 2_666
N1 Ni1 N3 89.21(14) . 2_666
O1W Ni1 N3 97.63(13) . 2_666
O1W Ni1 N3 82.37(13) 2_777 2_666
N1 Ni1 N3 89.21(14) 2_777 1_666
N1 Ni1 N3 90.79(14) . 1_666
O1W Ni1 N3 82.37(13) . 1_666
O1W Ni1 N3 97.63(13) 2_777 1_666
N3 Ni1 N3 180.000(2) 2_666 1_666
Ni1 O1W H1WB 119(5) . .
Ni1 O1W H1WA 129(4) . .
H1WB O1W H1WA 109(6) . .
C1 N1 C2 105.4(4) . .
C1 N1 Ni1 132.0(3) . .
C2 N1 Ni1 120.4(3) . .
C1 N2 C3 106.7(4) . .
C1 N2 C4 128.8(4) . .
C3 N2 C4 124.2(4) . .
C10 N3 N4 105.2(4) . .
C10 N3 Ni1 143.8(3) . 1_444
N4 N3 Ni1 110.3(3) . 1_444
N5 N4 N3 109.0(4) . .
N4 N5 N6 110.2(3) . .
C10 N6 N5 104.4(4) . .
N1 C1 N2 111.7(4) . .
N1 C1 H1A 124.1 . .
N2 C1 H1A 124.1 . .
C3 C2 N1 110.5(4) . .
C3 C2 H2A 124.8 . .
N1 C2 H2A 124.8 . .
C2 C3 N2 105.6(4) . .
C2 C3 H3A 127.2 . .
N2 C3 H3A 127.2 . .
C5 C4 C9 120.1(4) . .
C5 C4 N2 119.9(4) . .
C9 C4 N2 120.0(4) . .
C4 C5 C6 120.4(4) . .
C4 C5 H5A 119.8 . .
C6 C5 H5A 119.8 . .
C5 C6 C7 120.6(5) . .
C5 C6 H6A 119.7 . .
C7 C6 H6A 119.7 . .
C6 C7 C8 118.6(4) . .
C6 C7 C10 119.8(4) . .
C8 C7 C10 121.4(4) . .
C9 C8 C7 121.3(5) . .
C9 C8 H8A 119.4 . .
C7 C8 H8A 119.4 . .
C8 C9 C4 119.0(5) . .
C8 C9 H9A 120.5 . .
C4 C9 H9A 120.5 . .
N6 C10 N3 111.1(4) . .
N6 C10 C7 124.0(4) . .
N3 C10 C7 124.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.208(4) 2_777
Ni1 N1 2.208(4) .
Ni1 O1W 2.293(4) .
Ni1 O1W 2.293(4) 2_777
Ni1 N3 2.317(4) 2_666
Ni1 N3 2.317(4) 1_666
O1W H1WB 0.853(10) .
O1W H1WA 0.854(10) .
N1 C1 1.313(6) .
N1 C2 1.377(6) .
N2 C1 1.343(6) .
N2 C3 1.392(6) .
N2 C4 1.436(6) .
N3 C10 1.340(6) .
N3 N4 1.352(5) .
N3 Ni1 2.317(4) 1_444
N4 N5 1.299(5) .
N5 N6 1.355(6) .
N6 C10 1.338(6) .
C1 H1A 0.9300 .
C2 C3 1.341(7) .
C2 H2A 0.9300 .
C3 H3A 0.9300 .
C4 C5 1.374(7) .
C4 C9 1.398(7) .
C5 C6 1.381(7) .
C5 H5A 0.9300 .
C6 C7 1.385(7) .
C6 H6A 0.9300 .
C7 C8 1.393(7) .
C7 C10 1.478(6) .
C8 C9 1.377(7) .
C8 H8A 0.9300 .
C9 H9A 0.9300 .
