#------------------------------------------------------------------------------
#$Date: 2022-08-10 01:28:01 +0300 (Wed, 10 Aug 2022) $
#$Revision: 277176 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/52/7245285.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_7245285
loop_
_publ_author_name
'Li, Shuai'
'Han, Song-De'
'Zhao, Jiong-Peng'
'Liu, Fu-Chen'
_publ_section_title
;
 Quest for extended coordination networks from highly connected
 azido-bridged clusters
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00854H
_journal_year                    2022
_chemical_formula_moiety         'C36 H24 Co6 N24 O18, 1(O)'
_chemical_formula_sum            'C36 H26 Co6 N24 O19'
_chemical_formula_weight         1452.39
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-06-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-19 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.260(3)
_cell_length_b                   20.260(3)
_cell_length_c                   10.904(2)
_cell_measurement_reflns_used    5503
_cell_measurement_temperature    293.1
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      5.0
_cell_volume                     3876.1(11)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1121
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10959
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         3.483
_exptl_absorpt_coefficient_mu    1.980
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1514
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0585P)²+16.1232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1193
_reflns_number_total             1514
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00854h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        3876.3(14)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7245285
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Rigid bond restraints
 N3, N2, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.2
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C5(H5), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.53422(5) 0.24364(5) 0.24001(8) 0.0342(4) Uani 1 1 d . . . . .
O1 O 0.4659(3) 0.1259(3) 0.2470(4) 0.0451(13) Uani 1 1 d . . . . .
O3 O 0.3860(3) -0.1865(3) 0.3850(4) 0.0472(13) Uani 1 1 d . . . . .
O2 O 0.5224(3) 0.0954(2) 0.3952(4) 0.0410(12) Uani 1 1 d . . . . .
N4 N 0.3777(3) -0.1334(3) 0.3280(5) 0.0414(14) Uani 1 1 d . . . . .
N1 N 0.5947(3) 0.3668(3) 0.2304(5) 0.0347(13) Uani 1 1 d . U . . .
C1 C 0.4730(4) 0.0796(4) 0.3128(6) 0.0368(16) Uani 1 1 d . . . . .
C6 C 0.4260(4) -0.0585(4) 0.3505(6) 0.0355(16) Uani 1 1 d . . . . .
H6 H 0.464994 -0.044090 0.407459 0.043 Uiso 1 1 calc R U . . .
N2 N 0.5539(4) 0.3825(4) 0.1612(7) 0.0588(17) Uani 1 1 d . U . . .
C2 C 0.4178(4) -0.0035(4) 0.2897(6) 0.0384(16) Uani 1 1 d . . . . .
N3 N 0.5162(5) 0.3966(5) 0.0965(8) 0.091(3) Uani 1 1 d . U . . .
C3 C 0.3580(6) -0.0250(5) 0.2081(9) 0.085(3) Uani 1 1 d . . . . .
H3 H 0.352014 0.011508 0.165695 0.103 Uiso 1 1 calc R U . . .
C5 C 0.3188(6) -0.1552(5) 0.2502(8) 0.080(3) Uani 1 1 d . . . . .
H5 H 0.285293 -0.206701 0.236190 0.096 Uiso 1 1 calc R U . . .
C4 C 0.3081(7) -0.1006(5) 0.1910(12) 0.133(6) Uani 1 1 d . . . . .
H4 H 0.266505 -0.115799 0.139214 0.159 Uiso 1 1 calc R U . . .
O1W O 0.333333 0.666667 0.166667 0.265(18) Uani 1 6 d S TU 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'
Co Co 0.3494 0.9721 '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'
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
_geom_angle_publ_flag
O1 Co1 O2 82.55(19) . 17 ?
O1 Co1 N1 96.9(2) . 18_545 ?
O1 Co1 N1 174.05(19) . . ?
O1 Co1 N1 88.1(2) . 2_655 ?
O3 Co1 O1 89.30(19) 8_544 . ?
O3 Co1 O2 92.35(18) 8_544 17 ?
O3 Co1 N1 89.3(2) 8_544 . ?
O3 Co1 N1 173.4(2) 8_544 18_545 ?
O3 Co1 N1 93.8(2) 8_544 2_655 ?
O2 Co1 N1 168.75(19) 17 2_655 ?
O2 Co1 N1 91.7(2) 17 . ?
O2 Co1 N1 90.70(19) 17 18_545 ?
N1 Co1 N1 84.7(2) . 18_545 ?
N1 Co1 N1 97.8(3) . 2_655 ?
N1 Co1 N1 84.2(2) 2_655 18_545 ?
C1 O1 Co1 128.6(4) . . ?
N4 O3 Co1 122.5(4) . 6 ?
C1 O2 Co1 128.0(4) . 18_545 ?
O3 N4 C6 120.8(6) . . ?
O3 N4 C5 118.8(6) . . ?
C5 N4 C6 120.4(6) . . ?
Co1 N1 Co1 91.7(2) . 17 ?
Co1 N1 Co1 91.1(2) 3_665 17 ?
Co1 N1 Co1 141.7(3) . 3_665 ?
N2 N1 Co1 104.7(4) . . ?
N2 N1 Co1 113.8(5) . 17 ?
N2 N1 Co1 109.0(4) . 3_665 ?
O1 C1 O2 126.6(6) . . ?
O1 C1 C2 116.3(6) . . ?
O2 C1 C2 117.1(6) . . ?
N4 C6 H6 119.7 . . ?
N4 C6 C2 120.6(6) . . ?
C2 C6 H6 119.7 . . ?
N3 N2 N1 179.5(9) . . ?
C6 C2 C1 120.1(6) . . ?
C6 C2 C3 119.6(6) . . ?
C3 C2 C1 120.3(6) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 C2 118.8(8) . . ?
C4 C3 H3 120.6 . . ?
N4 C5 H5 120.1 . . ?
N4 C5 C4 119.9(8) . . ?
C4 C5 H5 120.1 . . ?
C3 C4 C5 120.6(9) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.077(5) . ?
Co1 O3 2.070(5) 8_544 ?
Co1 O2 2.126(4) 17 ?
Co1 N1 2.164(5) . ?
Co1 N1 2.193(6) 18_545 ?
Co1 N1 2.185(5) 2_655 ?
O1 C1 1.245(8) . ?
O3 N4 1.323(7) . ?
O2 C1 1.261(8) . ?
N4 C6 1.355(8) . ?
N4 C5 1.347(10) . ?
N1 N2 1.271(9) . ?
C1 C2 1.505(9) . ?
C6 H6 0.9300 . ?
C6 C2 1.377(9) . ?
N2 N3 1.174(9) . ?
C2 C3 1.386(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.361(12) . ?
C5 H5 0.9300 . ?
C5 C4 1.388(13) . ?
C4 H4 0.9300 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O1 C1 O2 3.8(10) . . . . ?
Co1 O1 C1 C2 -175.1(4) . . . . ?
Co1 O3 N4 C6 62.8(7) 6 . . . ?
Co1 O3 N4 C5 -115.0(7) 6 . . . ?
Co1 O2 C1 O1 -14.5(10) 18_545 . . . ?
Co1 O2 C1 C2 164.4(4) 18_545 . . . ?
O1 C1 C2 C6 174.1(6) . . . . ?
O1 C1 C2 C3 -6.5(11) . . . . ?
O3 N4 C6 C2 179.1(6) . . . . ?
O3 N4 C5 C4 178.9(10) . . . . ?
O2 C1 C2 C6 -4.9(9) . . . . ?
O2 C1 C2 C3 174.5(8) . . . . ?
N4 C6 C2 C1 -178.3(6) . . . . ?
N4 C6 C2 C3 2.3(11) . . . . ?
N4 C5 C4 C3 2(2) . . . . ?
C1 C2 C3 C4 -178.7(10) . . . . ?
C6 N4 C5 C4 1.1(15) . . . . ?
C6 C2 C3 C4 0.7(16) . . . . ?
C2 C3 C4 C5 -3(2) . . . . ?
C5 N4 C6 C2 -3.2(11) . . . . ?
