#------------------------------------------------------------------------------
#$Date: 2021-02-27 07:59:47 +0200 (Sat, 27 Feb 2021) $
#$Revision: 262298 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/37/2243763.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243763
loop_
_publ_author_name
'Mirzaei, Masoud'
'Bazargan, Maryam'
'Ebtehaj, Pouria'
'Mague, Joel T.'
_publ_section_title
;
 A redetermination of the structure and Hirshfeld surface analysis of
 poly[diaquadi-μ-hydroxido-tetrakis(μ-nicotinato
 N-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-μ-hydroxido-tetrakis(μ-pyridine-3-carboxylato
N-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
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018/1 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_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       'φ and ω 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
;
(SADABS; Krause et al., 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/[σ²(Fo²)+(0.0347P)²+0.5335P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            jq2004sup1.cif
_cod_data_source_block           I
_cod_database_code               2243763
_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.
;
_shelx_estimated_absorpt_t_min   0.523
_shelx_estimated_absorpt_t_max   0.618
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.55161(3) 0.76197(2) 0.22674(2) 0.01203(6) Uani d 1 . .
Cu Cu2 0.500000 0.500000 0.000000 0.01188(7) Uani d 1 . .
O O1 0.44050(18) 0.71790(14) 0.36494(13) 0.0175(2) Uani d 1 . .
O O2 0.2406(2) 0.47108(14) 0.27160(14) 0.0245(3) Uani d 1 . .
O O3 0.22121(19) 0.36322(14) 0.73304(14) 0.0189(2) Uani d 1 . .
O O4 0.38030(18) 0.32089(13) 0.05837(12) 0.0146(2) Uani d 1 . .
O O5 0.35598(18) 0.12662(13) -0.09985(12) 0.0154(2) Uani d 1 . .
O O6 0.09294(18) 0.09404(14) 0.36357(12) 0.0166(2) Uani d 1 . .
O O7 0.35789(17) 0.59314(13) 0.07123(12) 0.0126(2) Uani d 1 . .
H H7A 0.308(3) 0.534(2) 0.110(2) 0.029(6) Uiso d 1 . .
O O8 0.74783(18) 0.94425(13) 0.37813(12) 0.0152(2) Uani d 1 . .
H H8A 0.788(4) 0.931(3) 0.4591(16) 0.041(8) Uiso d 1 . .
H H8B 0.848(3) 0.981(3) 0.362(3) 0.035(7) Uiso d 1 . .
N N1 0.2291(2) 0.47710(16) 0.67356(14) 0.0135(3) Uani d 1 . .
N N2 0.13829(19) 0.03830(15) 0.26216(14) 0.0119(2) Uani d 1 . .
C C1 0.3226(2) 0.59140(18) 0.36527(17) 0.0138(3) Uani d 1 . .
C C2 0.2845(2) 0.59731(18) 0.49796(16) 0.0122(3) Uani d 1 . .
C C3 0.2577(2) 0.47220(18) 0.55191(17) 0.0136(3) Uani d 1 . .
H H3 0.259212 0.383122 0.504107 0.016 Uiso calc 1 . .
C C4 0.2081(2) 0.59753(19) 0.73601(17) 0.0155(3) Uani d 1 . .
H H4 0.178573 0.595901 0.816802 0.019 Uiso calc 1 . .
C C5 0.2293(3) 0.7225(2) 0.68303(17) 0.0171(3) Uani d 1 . .
H H5 0.212768 0.806108 0.726578 0.020 Uiso calc 1 . .
C C6 0.2751(2) 0.72616(19) 0.56552(17) 0.0152(3) Uani d 1 . .
H H6 0.299241 0.814314 0.532209 0.018 Uiso calc 1 . .
C C7 0.3409(2) 0.18427(17) 0.00894(16) 0.0111(3) Uani d 1 . .
C C8 0.2615(2) 0.07659(17) 0.08634(15) 0.0109(3) Uani d 1 . .
C C9 0.2181(2) 0.13269(17) 0.19519(16) 0.0117(3) Uani d 1 . .
H H9 0.244784 0.237223 0.221998 0.014 Uiso calc 1 . .
C C10 0.0996(2) -0.11165(18) 0.22703(17) 0.0143(3) Uani d 1 . .
H H10 0.043095 -0.176028 0.275773 0.017 Uiso calc 1 . .
C C11 0.1424(2) -0.17042(18) 0.12053(18) 0.0160(3) Uani d 1 . .
H H11 0.115782 -0.275146 0.096237 0.019 Uiso calc 1 . .
C C12 0.2246(2) -0.07639(18) 0.04886(17) 0.0141(3) Uani d 1 . .
H H12 0.254937 -0.115727 -0.024337 0.017 Uiso calc 1 . .
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'
Cu Cu 0.3201 1.2651 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O7 Cu1 O8 . . 176.16(5) ?
O7 Cu1 O1 . . 97.79(5) ?
O8 Cu1 O1 . . 84.60(5) ?
O7 Cu1 O5 . 2_665 92.38(5) ?
O8 Cu1 O5 . 2_665 84.42(5) ?
O1 Cu1 O5 . 2_665 158.98(5) ?
O7 Cu1 O3 . 2_666 89.57(5) ?
O8 Cu1 O3 . 2_666 92.82(5) ?
O1 Cu1 O3 . 2_666 103.19(5) ?
O5 Cu1 O3 2_665 2_666 95.20(5) ?
O7 Cu2 O7 2_665 . 180.0 ?
O7 Cu2 O4 2_665 . 92.31(5) ?
O7 Cu2 O4 . . 87.69(5) ?
O7 Cu2 O4 2_665 2_665 87.69(5) ?
O7 Cu2 O4 . 2_665 92.31(5) ?
O4 Cu2 O4 . 2_665 180.00(8) ?
C1 O1 Cu1 . . 128.46(11) ?
N1 O3 Cu1 . 2_666 125.82(9) ?
C7 O4 Cu2 . . 129.98(10) ?
C7 O5 Cu1 . 2_665 125.97(10) ?
Cu1 O7 Cu2 . . 106.58(6) ?
Cu1 O7 H7A . . 102.7(18) ?
Cu2 O7 H7A . . 104.7(18) ?
Cu1 O8 H8A . . 115(2) ?
Cu1 O8 H8B . . 110.4(19) ?
H8A O8 H8B . . 106(3) ?
O3 N1 C4 . . 118.78(13) ?
O3 N1 C3 . . 120.31(14) ?
C4 N1 C3 . . 120.91(14) ?
O6 N2 C9 . . 118.69(13) ?
O6 N2 C10 . . 119.75(13) ?
C9 N2 C10 . . 121.54(14) ?
O2 C1 O1 . . 127.26(15) ?
O2 C1 C2 . . 119.22(14) ?
O1 C1 C2 . . 113.52(14) ?
C3 C2 C6 . . 119.94(14) ?
C3 C2 C1 . . 119.12(14) ?
C6 C2 C1 . . 120.94(14) ?
N1 C3 C2 . . 119.92(15) ?
N1 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
N1 C4 C5 . . 120.41(15) ?
N1 C4 H4 . . 119.8 ?
C5 C4 H4 . . 119.8 ?
C4 C5 C6 . . 119.99(15) ?
C4 C5 H5 . . 120.0 ?
C6 C5 H5 . . 120.0 ?
C5 C6 C2 . . 118.49(15) ?
C5 C6 H6 . . 120.8 ?
C2 C6 H6 . . 120.8 ?
O4 C7 O5 . . 127.42(14) ?
O4 C7 C8 . . 116.01(13) ?
O5 C7 C8 . . 116.56(14) ?
C12 C8 C9 . . 119.83(14) ?
C12 C8 C7 . . 121.94(14) ?
C9 C8 C7 . . 118.19(14) ?
N2 C9 C8 . . 119.81(14) ?
N2 C9 H9 . . 120.1 ?
C8 C9 H9 . . 120.1 ?
N2 C10 C11 . . 120.03(14) ?
N2 C10 H10 . . 120.0 ?
C11 C10 H10 . . 120.0 ?
C10 C11 C12 . . 120.01(15) ?
C10 C11 H11 . . 120.0 ?
C12 C11 H11 . . 120.0 ?
C11 C12 C8 . . 118.77(15) ?
C11 C12 H12 . . 120.6 ?
C8 C12 H12 . . 120.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 O7 . 1.9003(12) ?
Cu1 O8 . 1.9539(12) ?
Cu1 O1 . 1.9542(12) ?
Cu1 O5 2_665 1.9911(12) ?
Cu1 O3 2_666 2.4208(13) ?
Cu2 O7 2_665 1.9240(11) ?
Cu2 O7 . 1.9240(11) ?
Cu2 O4 . 1.9687(11) ?
Cu2 O4 2_665 1.9688(11) ?
O1 C1 . 1.276(2) ?
O2 C1 . 1.232(2) ?
O3 N1 . 1.3270(17) ?
O4 C7 . 1.2541(19) ?
O5 C7 . 1.2638(19) ?
O6 N2 . 1.3381(17) ?
O7 H7A . 0.819(10) ?
O8 H8A . 0.833(10) ?
O8 H8B . 0.836(10) ?
N1 C4 . 1.354(2) ?
N1 C3 . 1.362(2) ?
N2 C9 . 1.3462(19) ?
N2 C10 . 1.360(2) ?
C1 C2 . 1.513(2) ?
C2 C3 . 1.386(2) ?
C2 C6 . 1.396(2) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.379(2) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.395(2) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 C8 . 1.507(2) ?
C8 C12 . 1.393(2) ?
C8 C9 . 1.394(2) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.381(2) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.390(2) ?
C11 H11 . 0.9500 ?
C12 H12 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O7 H7A O2 . 0.819(10) 2.037(14) 2.8057(17) 156(2) yes
O8 H8A O6 2_666 0.833(10) 1.840(11) 2.6684(17) 173(3) yes
O8 H8B O6 1_665 0.836(10) 1.875(11) 2.6976(18) 168(3) yes
C9 H9 O2 . 0.95 2.28 3.216(2) 168 yes
C10 H10 O3 2_556 0.95 2.23 3.079(2) 148 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cu1 O3 N1 C4 2_666 . . . -133.95(13) ?
Cu1 O3 N1 C3 2_666 . . . 46.08(19) ?
Cu1 O1 C1 O2 . . . . -6.2(3) ?
Cu1 O1 C1 C2 . . . . 174.06(10) ?
O2 C1 C2 C3 . . . . 35.0(2) ?
O1 C1 C2 C3 . . . . -145.22(15) ?
O2 C1 C2 C6 . . . . -144.61(17) ?
O1 C1 C2 C6 . . . . 35.1(2) ?
O3 N1 C3 C2 . . . . -173.87(14) ?
C4 N1 C3 C2 . . . . 6.2(2) ?
C6 C2 C3 N1 . . . . -2.3(2) ?
C1 C2 C3 N1 . . . . 178.07(14) ?
O3 N1 C4 C5 . . . . 175.41(15) ?
C3 N1 C4 C5 . . . . -4.6(2) ?
N1 C4 C5 C6 . . . . -0.8(3) ?
C4 C5 C6 C2 . . . . 4.5(3) ?
C3 C2 C6 C5 . . . . -2.9(2) ?
C1 C2 C6 C5 . . . . 176.69(15) ?
Cu2 O4 C7 O5 . . . . -5.8(3) ?
Cu2 O4 C7 C8 . . . . 175.93(10) ?
Cu1 O5 C7 O4 2_665 . . . 0.0(2) ?
Cu1 O5 C7 C8 2_665 . . . 178.24(10) ?
O4 C7 C8 C12 . . . . -175.48(15) ?
O5 C7 C8 C12 . . . . 6.0(2) ?
O4 C7 C8 C9 . . . . 6.8(2) ?
O5 C7 C8 C9 . . . . -171.71(14) ?
O6 N2 C9 C8 . . . . -178.18(13) ?
C10 N2 C9 C8 . . . . 0.5(2) ?
C12 C8 C9 N2 . . . . -0.9(2) ?
C7 C8 C9 N2 . . . . 176.91(13) ?
O6 N2 C10 C11 . . . . 178.72(14) ?
C9 N2 C10 C11 . . . . 0.1(2) ?
N2 C10 C11 C12 . . . . -0.2(2) ?
C10 C11 C12 C8 . . . . -0.2(2) ?
C9 C8 C12 C11 . . . . 0.8(2) ?
C7 C8 C12 C11 . . . . -176.96(14) ?

_cod_database_fobs_code 2243763
