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_7245286
_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         'C24 H16 Co4 N19 O12, H3 O, 4(O)'
_chemical_formula_sum            'C24 H27 Co4 N19 O17'
_chemical_formula_weight         1089.37
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_formula_units_Z            2
_cell_length_a                   13.702(3)
_cell_length_b                   13.702(3)
_cell_length_c                   11.139(2)
_cell_measurement_reflns_used    5503
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      5.0
_cell_volume                     2091.3(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.2468
_diffrn_reflns_av_unetI/netI     0.1308
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16424
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.706
_diffrn_reflns_theta_max         24.706
_diffrn_reflns_theta_min         2.973
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         1789
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1812
_refine_ls_R_factor_gt           0.0987
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+2.3734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1047
_reflns_number_total             1789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00854h2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2091.3(10)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7245286
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.734
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
2. Others
 Fixed Sof: H1W(0.75) O2W(0.5) O3W(0.5)
3.a Riding coordinates:
 O1W(H1W)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
;
_shelx_res_checksum              18044
_shelx_hkl_checksum              14639
_olex2_submission_special_instructions 'No special instructions were received'