Quest for extended coordination networks from highly connected azido-bridged clusters
Li, Shuai; Han, Song-De; Zhao, Jiong-Peng; Liu, Fu-Chen; CrystEngComm  (2022) –; doi:10.1039/D2CE00854H

data_7245285
_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       '\w 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/[\s^2^(Fo^2^)+(0.0585P)^2^+16.1232P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;
_shelx_res_checksum              26811
_shelx_hkl_checksum              28760
_olex2_submission_special_instructions 'No special instructions were received'