#------------------------------------------------------------------------------
#$Date: 2019-05-01 05:01:09 +0300 (Wed, 01 May 2019) $
#$Revision: 214881 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/26/7232697.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_7232697
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         '2(C20 H15 Cl Co2 N12 O), 7(H2 O)'
_chemical_formula_sum            'C40 H44 Cl2 Co4 N24 O9'
_chemical_formula_weight         1311.61
_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
_audit_update_record
;
2018-09-04 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.333(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.117(4)
_cell_length_b                   6.5151(8)
_cell_length_c                   25.559(3)
_cell_measurement_reflns_used    16564
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.38
_cell_volume                     4910.7(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16564
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.519
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.308
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4364
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0471
_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)+(0.0820P)²+20.6284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                3521
_reflns_number_total             4364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ra01327j2.cif
_cod_data_source_block           1
_cod_original_cell_volume        4910.6(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7232697
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
Co1 Co 0.091807(18) 0.03289(8) 0.49393(2) 0.00773(18) Uani 1 1 d .
Co2 Co -0.008274(18) 0.20281(8) 0.46460(2) 0.00696(17) Uani 1 1 d .
Cl1 Cl 0.02314(3) 0.02044(16) 0.40095(5) 0.0134(3) Uani 1 1 d .
N1 N 0.08312(11) 0.3686(5) 0.48467(16) 0.0098(8) Uani 1 1 d .
N2 N 0.04238(11) 0.4351(5) 0.48052(15) 0.0085(7) Uani 1 1 d .
N3 N 0.04362(11) 0.6320(5) 0.49018(15) 0.0086(7) Uani 1 1 d .
N4 N 0.08553(11) 0.7009(5) 0.50018(15) 0.0091(7) Uani 1 1 d .
C3 C 0.33368(16) 0.5408(9) 0.6114(2) 0.0267(12) Uani 1 1 d .
H3B H 0.3302 0.5573 0.6456 0.032 Uiso 1 1 calc R
C2 C 0.37294(17) 0.5298(9) 0.6043(2) 0.0244(12) Uani 1 1 d .
H2A H 0.4017 0.5393 0.6334 0.029 Uiso 1 1 calc R
N6 N 0.36431(12) 0.5024(5) 0.54765(17) 0.0117(8) Uani 1 1 d .
C1 C 0.31982(15) 0.5019(6) 0.5209(2) 0.0118(9) Uani 1 1 d .
H1A H 0.3044 0.4888 0.4817 0.014 Uiso 1 1 calc R
C20 C -0.08296(18) 0.5222(9) 0.3098(2) 0.0300(13) Uani 1 1 d .
H20 H -0.0861 0.6148 0.2808 0.036 Uiso 1 1 calc R
C21 C -0.04572(17) 0.4976(8) 0.3591(2) 0.0234(12) Uani 1 1 d .
H21 H -0.0189 0.5719 0.3698 0.028 Uiso 1 1 calc R
N8 N -0.05438(12) 0.3435(6) 0.39077(16) 0.0116(8) Uani 1 1 d .
C22 C -0.09622(15) 0.2815(7) 0.3600(2) 0.0165(10) Uani 1 1 d .
H22 H -0.1110 0.1782 0.3710 0.020 Uiso 1 1 calc R
N12 N -0.31097(12) 0.4241(6) 0.09746(17) 0.0154(8) Uani 1 1 d .
N11 N -0.35592(12) 0.4036(6) 0.07681(17) 0.0129(8) Uani 1 1 d .
N10 N -0.36919(13) 0.3134(6) 0.11318(18) 0.0202(9) Uani 1 1 d .
N9 N -0.33222(14) 0.2766(7) 0.16071(18) 0.0237(10) Uani 1 1 d .
N5 N 0.29963(12) 0.5229(5) 0.55786(17) 0.0119(8) Uani 1 1 d .
C4 C 0.25142(14) 0.5264(6) 0.5423(2) 0.0108(9) Uani 1 1 d U
C9 C 0.22229(15) 0.4821(7) 0.4867(2) 0.0131(9) Uani 1 1 d .
H3A H 0.2339 0.4508 0.4597 0.016 Uiso 1 1 calc R
C8 C 0.17607(14) 0.4844(7) 0.4716(2) 0.0118(9) Uani 1 1 d .
H4A H 0.1566 0.4527 0.4345 0.014 Uiso 1 1 calc R
C7 C 0.15839(14) 0.5336(6) 0.5114(2) 0.0099(9) Uani 1 1 d .
C6 C 0.18768(15) 0.5811(7) 0.5662(2) 0.0167(10) Uani 1 1 d .
H6A H 0.1759 0.6172 0.5928 0.020 Uiso 1 1 calc R
C5 C 0.23451(15) 0.5764(8) 0.5826(2) 0.0165(10) Uani 1 1 d .
H7A H 0.2539 0.6063 0.6199 0.020 Uiso 1 1 calc R
C10 C 0.10909(14) 0.5354(6) 0.49734(18) 0.0087(9) Uani 1 1 d .
N7 N -0.11473(13) 0.3857(7) 0.31093(17) 0.0211(9) Uani 1 1 d .
C17 C -0.16040(16) 0.3634(8) 0.2690(2) 0.0227(11) Uani 1 1 d .
C18 C -0.19384(17) 0.2909(8) 0.2854(2) 0.0220(11) Uani 1 1 d .
H11A H -0.1866 0.2503 0.3229 0.026 Uiso 1 1 calc R
C19 C -0.23824(16) 0.2789(8) 0.2457(2) 0.0218(11) Uani 1 1 d .
H12A H -0.2606 0.2282 0.2567 0.026 Uiso 1 1 calc R
C16 C -0.17098(17) 0.4174(9) 0.2129(2) 0.0282(12) Uani 1 1 d .
H13A H -0.1483 0.4605 0.2015 0.034 Uiso 1 1 calc R
C15 C -0.21516(17) 0.4070(9) 0.1741(2) 0.0273(12) Uani 1 1 d .
H14A H -0.2222 0.4447 0.1365 0.033 Uiso 1 1 calc R
C14 C -0.24970(16) 0.3410(8) 0.1902(2) 0.0209(11) Uani 1 1 d .
C23 C -0.29710(16) 0.3450(8) 0.1496(2) 0.0187(10) Uani 1 1 d .
O O 0.04424(9) 0.0515(4) 0.52993(13) 0.0087(6) Uani 1 1 d .
H0A H 0.0555 0.1310 0.5654 0.010 Uiso 1 1 calc R
O1W O 0.05068(19) 0.3271(8) 0.3089(2) 0.0634(15) Uani 1 1 d .
H1WB H 0.0776 0.3637 0.3296 0.076 Uiso 1 1 d R
H1WC H 0.0385 0.2790 0.3304 0.076 Uiso 1 1 d R
O2W O 0.14861(18) 0.1086(8) 0.7624(2) 0.0585(14) Uani 1 1 d .
H2WC H 0.1530 0.1404 0.7327 0.070 Uiso 1 1 d R
H2WD H 0.1209 0.0753 0.7523 0.070 Uiso 1 1 d R
O3W O 0.0000 0.6835(10) 0.2500 0.0518(18) Uani 1 2 d S
H3WA H 0.0195 0.7488 0.2418 0.062 Uiso 0.50 1 d PR
H3WB H -0.0180 0.6321 0.2186 0.062 Uiso 0.50 1 d PR
O4W O 0.05380(15) 0.0098(7) 0.2328(2) 0.0429(11) Uani 1 1 d .
H4WC H 0.0612 0.1167 0.2535 0.07(3) Uiso 1 1 d R
H4WD H 0.0324 0.0183 0.2000 0.07(3) Uiso 1 1 d R
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'
B B 0.0013 0.0007 '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'
Cl Cl 0.1484 0.1585 '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
O Co1 N6 175.01(13) . 7_556
O Co1 N11 88.67(13) . 8_556
N6 Co1 N11 95.81(14) 7_556 8_556
O Co1 N4 85.40(12) . 1_545
N6 Co1 N4 91.64(13) 7_556 1_545
N11 Co1 N4 100.18(14) 8_556 1_545
O Co1 N1 84.59(12) . .
N6 Co1 N1 97.87(13) 7_556 .
N11 Co1 N1 86.06(14) 8_556 .
N4 Co1 N1 168.08(13) 1_545 .
O Co1 Cl1 84.10(9) . .
N6 Co1 Cl1 91.80(11) 7_556 .
N11 Co1 Cl1 168.62(10) 8_556 .
N4 Co1 Cl1 88.02(10) 1_545 .
N1 Co1 Cl1 84.52(10) . .
O Co2 O 82.12(12) 5_556 .
O Co2 N8 101.45(13) 5_556 .
O Co2 N8 170.12(13) . .
O Co2 N2 164.24(13) 5_556 .
O Co2 N2 82.51(12) . .
N8 Co2 N2 94.28(14) . .
O Co2 N3 86.42(12) 5_556 5_566
O Co2 N3 103.43(13) . 5_566
N8 Co2 N3 86.06(14) . 5_566
N2 Co2 N3 93.77(13) . 5_566
O Co2 Cl1 92.48(9) 5_556 .
O Co2 Cl1 83.73(9) . .
N8 Co2 Cl1 86.89(11) . .
N2 Co2 Cl1 89.30(10) . .
N3 Co2 Cl1 172.50(10) 5_566 .
Co1 Cl1 Co2 78.53(4) . .
C10 N1 N2 104.7(3) . .
C10 N1 Co1 138.1(3) . .
N2 N1 Co1 114.0(3) . .
N3 N2 N1 110.3(3) . .
N3 N2 Co2 134.1(3) . .
N1 N2 Co2 115.5(3) . .
N2 N3 N4 108.5(3) . .
N2 N3 Co2 126.8(3) . 5_566
N4 N3 Co2 115.1(3) . 5_566
C10 N4 N3 105.5(3) . .
C10 N4 Co1 136.5(3) . 1_565
N3 N4 Co1 115.6(3) . 1_565
C2 C3 N5 106.2(5) . .
C2 C3 H3B 126.9 . .
N5 C3 H3B 126.9 . .
C3 C2 N6 109.9(4) . .
C3 C2 H2A 125.0 . .
N6 C2 H2A 125.0 . .
C1 N6 C2 105.8(4) . .
C1 N6 Co1 123.2(3) . 7_556
C2 N6 Co1 131.0(3) . 7_556
N6 C1 N5 111.1(4) . .
N6 C1 H1A 124.4 . .
N5 C1 H1A 124.4 . .
C21 C20 N7 107.1(4) . .
C21 C20 H20 126.4 . .
N7 C20 H20 126.4 . .
C20 C21 N8 108.7(4) . .
C20 C21 H21 125.7 . .
N8 C21 H21 125.7 . .
C22 N8 C21 105.4(4) . .
C22 N8 Co2 126.3(3) . .
C21 N8 Co2 127.6(3) . .
N8 C22 N7 111.8(4) . .
N8 C22 H22 124.1 . .
N7 C22 H22 124.1 . .
C23 N12 N11 103.8(4) . .
N10 N11 N12 111.8(4) . .
N10 N11 Co1 116.0(3) . 8_455
N12 N11 Co1 132.0(3) . 8_455
N11 N10 N9 107.7(4) . .
N10 N9 C23 105.3(4) . .
C1 N5 C3 107.0(4) . .
C1 N5 C4 124.9(4) . .
C3 N5 C4 128.1(4) . .
C5 C4 C9 120.6(4) . .
C5 C4 N5 119.8(4) . .
C9 C4 N5 119.7(4) . .
C8 C9 C4 119.9(4) . .
C8 C9 H3A 120.0 . .
C4 C9 H3A 120.0 . .
C9 C8 C7 120.5(4) . .
C9 C8 H4A 119.8 . .
C7 C8 H4A 119.8 . .
C6 C7 C8 119.0(4) . .
C6 C7 C10 118.6(4) . .
C8 C7 C10 122.4(4) . .
C7 C6 C5 121.5(4) . .
C7 C6 H6A 119.2 . .
C5 C6 H6A 119.2 . .
C4 C5 C6 118.5(4) . .
C4 C5 H7A 120.7 . .
C6 C5 H7A 120.7 . .
N1 C10 N4 111.0(4) . .
N1 C10 C7 124.1(4) . .
N4 C10 C7 124.6(4) . .
C22 N7 C20 107.0(4) . .
C22 N7 C17 126.1(4) . .
C20 N7 C17 126.9(4) . .
C16 C17 C18 120.0(5) . .
C16 C17 N7 120.4(5) . .
C18 C17 N7 119.6(5) . .
C17 C18 C19 119.7(5) . .
C17 C18 H11A 120.2 . .
C19 C18 H11A 120.2 . .
C14 C19 C18 121.0(5) . .
C14 C19 H12A 119.5 . .
C18 C19 H12A 119.5 . .
C15 C16 C17 119.7(5) . .
C15 C16 H13A 120.1 . .
C17 C16 H13A 120.1 . .
C16 C15 C14 121.2(5) . .
C16 C15 H14A 119.4 . .
C14 C15 H14A 119.4 . .
C19 C14 C15 118.3(4) . .
C19 C14 C23 120.9(4) . .
C15 C14 C23 120.7(5) . .
N12 C23 N9 111.4(4) . .
N12 C23 C14 124.0(4) . .
N9 C23 C14 124.6(4) . .
Co2 O Co1 121.01(14) 5_556 .
Co2 O Co2 97.88(12) 5_556 .
Co1 O Co2 100.14(13) . .
Co2 O H0A 112.0 5_556 .
Co1 O H0A 112.0 . .
Co2 O H0A 112.0 . .
H1WB O1W H1WC 108.4 . .
H2WC O2W H2WD 108.4 . .
H3WA O3W H3WB 104.8 . .
H4WC O4W H4WD 118.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O 2.076(3) .
Co1 N6 2.087(4) 7_556
Co1 N11 2.159(4) 8_556
Co1 N4 2.184(4) 1_545
Co1 N1 2.206(4) .
Co1 Cl1 2.5232(12) .
Co2 O 2.056(3) 5_556
Co2 O 2.091(3) .
Co2 N8 2.093(4) .
Co2 N2 2.140(3) .
Co2 N3 2.196(4) 5_566
Co2 Cl1 2.5251(12) .
N1 C10 1.329(6) .
N1 N2 1.342(5) .
N2 N3 1.304(5) .
N3 N4 1.344(5) .
N3 Co2 2.196(4) 5_566
N4 C10 1.336(5) .
N4 Co1 2.184(4) 1_565
C3 C2 1.345(7) .
C3 N5 1.377(6) .
C3 H3B 0.9300 .
C2 N6 1.373(6) .
C2 H2A 0.9300 .
N6 C1 1.317(6) .
N6 Co1 2.087(4) 7_556
C1 N5 1.348(6) .
C1 H1A 0.9300 .
C20 C21 1.360(7) .
C20 N7 1.362(7) .
C20 H20 0.9300 .
C21 N8 1.385(6) .
C21 H21 0.9300 .
N8 C22 1.323(6) .
C22 N7 1.340(6) .
C22 H22 0.9300 .
N12 C23 1.329(6) .
N12 N11 1.333(5) .
N11 N10 1.306(6) .
N11 Co1 2.159(4) 8_455
N10 N9 1.342(6) .
N9 C23 1.344(6) .
N5 C4 1.438(5) .
C4 C5 1.380(7) .
C4 C9 1.388(7) .
C9 C8 1.378(6) .
C9 H3A 0.9300 .
C8 C7 1.383(6) .
C8 H4A 0.9300 .
C7 C6 1.378(7) .
C7 C10 1.479(6) .
C6 C5 1.392(6) .
C6 H6A 0.9300 .
C5 H7A 0.9300 .
N7 C17 1.441(6) .
C17 C16 1.381(7) .
C17 C18 1.382(7) .
C18 C19 1.386(7) .
C18 H11A 0.9300 .
C19 C14 1.378(7) .
C19 H12A 0.9300 .
C16 C15 1.374(7) .
C16 H13A 0.9300 .
C15 C14 1.394(7) .
C15 H14A 0.9300 .
C14 C23 1.464(7) .
O Co2 2.056(3) 5_556
O H0A 0.9800 .
O1W H1WB 0.8502 .
O1W H1WC 0.8500 .
O2W H2WC 0.8499 .
O2W H2WD 0.8501 .
O3W H3WA 0.8500 .
O3W H3WB 0.8501 .
O4W H4WC 0.8499 .
O4W H4WD 0.8499 .
