A redetermination of the structure and Hirshfeld surface analysis of poly[diaquadi-μ-hydroxido-tetrakis(μ-nicotinato <i>N</i>-oxide)tricopper(II)]
Mirzaei, Masoud; Bazargan, Maryam; Ebtehaj, Pouria; Mague, Joel T.; Acta Crystallographica Section E 77 (2021) 309–313; doi:10.1107/S2056989021002000

data_2243763
_publ_section_title
;
 A redetermination of the structure and Hirshfeld surface analysis of
 poly[diaquadi-\m-hydroxido-tetrakis(\m-nicotinato
 <i>N</i>-oxide)tricopper(II)]
;
_journal_coeditor_code           JQ2004
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              309
_journal_page_last               313
_journal_paper_doi               10.1107/S2056989021002000
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Cu3 (C6 H4 N1 O3)4 (O H)2 (H2 O1)2]'
_chemical_formula_moiety         'C24 H22 Cu3 N4 O16'
_chemical_formula_sum            'C24 H22 Cu3 N4 O16'
_chemical_formula_weight         813.07
_chemical_name_systematic
;
Poly[diaquadi-\m-hydroxido-tetrakis(\m-pyridine-3-carboxylato
<i>N</i>-oxide)tricopper(II)]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                97.016(3)
_cell_angle_beta                 110.701(3)
_cell_angle_gamma                109.049(3)
_cell_formula_units_Z            1
_cell_length_a                   7.8669(17)
_cell_length_b                   9.710(2)
_cell_length_c                   10.424(2)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      29.1428
_cell_measurement_theta_min      2.3037
_cell_volume                     678.2(2)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12893
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.147
_diffrn_reflns_theta_min         2.168
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.422
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             409
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3592
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0347P)^2^+0.5335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                3390
_reflns_number_total             3592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jq2004sup1.cif
_cod_data_source_block           I
_cod_database_code               2243763
_shelx_estimated_absorpt_t_min   0.523
_shelx_estimated_absorpt_t_max   0.618
_shelx_hkl_checksum              13812
_shelx_res_checksum              63661
_cod_database_fobs_code 2243763