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#$Date: 2023-06-05 07:45:09 +0300 (Mon, 05 Jun 2023) $
#$Revision: 284297 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/24/7062434.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_7062434
loop_
_publ_author_name
'Klongdee, Fatima'
'Sasada, Yuto'
'Nakano, Motohiro'
'Chainok, Kittipong'
'Youngme, Sujittra'
'Boonmak, Jaursup'
_publ_section_title
;
 Synthesis, X-ray structures, and magnetic properties of seven polynuclear
 Cu(ii) complexes containing pyrazole-3,5-dicarboxylate with various
 ancillary ligands
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9669
_journal_page_last               9680
_journal_paper_doi               10.1039/D3NJ00821E
_journal_volume                  47
_journal_year                    2023
_chemical_formula_sum            'C20 H20 Cu2 N8 O10'
_chemical_formula_weight         659.52
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-04-18 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                76.802(13)
_cell_angle_beta                 82.568(14)
_cell_angle_gamma                72.681(14)
_cell_formula_units_Z            1
_cell_length_a                   6.338(3)
_cell_length_b                   7.373(3)
_cell_length_c                   13.513(6)
_cell_measurement_reflns_used    4691
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.5295
_cell_measurement_theta_min      2.9545
_cell_volume                     585.6(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       BrukerAPEX2
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Bruker D8 QUEST PHOTON 100
;
_diffrn_measurement_method       '\fandω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15904
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         2.954
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_description       block
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2057
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0206P)²+0.6592P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1677
_reflns_number_total             2057
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj00821e2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7062429--7062435.cif.'
_cod_original_cell_volume        585.6(4)
_cod_database_code               7062434
_shelx_shelxl_version_number     2014/7
_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   0.848
_shelx_estimated_absorpt_t_max   0.945
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Cu1 Cu 1.15790(6) 0.40122(5) 0.62659(3) 0.02147(13) Uani 1 1 d . . . . .
O1 O 1.1610(3) 0.1512(3) 0.72801(15) 0.0239(5) Uani 1 1 d . . . . .
O2 O 1.0029(4) -0.0909(3) 0.76879(15) 0.0286(5) Uani 1 1 d . . . . .
O3 O 0.6057(3) 0.5012(3) 0.33343(14) 0.0235(5) Uani 1 1 d . . . . .
O4 O 0.4488(4) 0.2580(3) 0.37641(17) 0.0351(6) Uani 1 1 d . . . . .
O5 O 0.9105(4) 0.5761(3) 0.73528(17) 0.0283(5) Uani 1 1 d D . . . .
N1 N 0.9563(4) 0.3123(3) 0.56815(17) 0.0222(6) Uani 1 1 d . . . . .
N2 N 0.8402(4) 0.3867(3) 0.48608(17) 0.0224(6) Uani 1 1 d . . . . .
N3 N 0.5062(5) 0.6313(4) 0.1363(2) 0.0374(7) Uani 1 1 d . . . . .
H3 H 0.4999 0.5750 0.1993 0.045 Uiso 1 1 calc R U . . .
N4 N 0.5346(4) 0.9090(4) -0.16090(19) 0.0311(7) Uani 1 1 d . . . . .
H4A H 0.4147 0.9643 -0.1920 0.037 Uiso 1 1 calc R U . . .
H4B H 0.6604 0.9149 -0.1920 0.037 Uiso 1 1 calc R U . . .
C1 C 1.0286(5) 0.0588(4) 0.7117(2) 0.0196(7) Uani 1 1 d . . . . .
C2 C 0.9047(5) 0.1504(4) 0.6182(2) 0.0193(7) Uani 1 1 d . . . . .
C3 C 0.7480(5) 0.1173(4) 0.5656(2) 0.0203(7) Uani 1 1 d . . . . .
H3A H 0.6826 0.0159 0.5824 0.024 Uiso 1 1 calc R U . . .
C4 C 0.7127(5) 0.2711(4) 0.4823(2) 0.0189(7) Uani 1 1 d . . . . .
C5 C 0.5770(5) 0.3429(4) 0.3921(2) 0.0203(7) Uani 1 1 d . . . . .
C6 C 0.7020(6) 0.6380(5) 0.0878(3) 0.0380(9) Uani 1 1 d . . . . .
H6 H 0.8298 0.5819 0.1231 0.046 Uiso 1 1 calc R U . . .
C7 C 0.7189(6) 0.7242(5) -0.0111(2) 0.0317(8) Uani 1 1 d . . . . .
H7 H 0.8575 0.7241 -0.0437 0.038 Uiso 1 1 calc R U . . .
C8 C 0.5255(5) 0.8151(4) -0.0654(2) 0.0250(7) Uani 1 1 d . . . . .
C9 C 0.3223(5) 0.8022(5) -0.0118(2) 0.0317(8) Uani 1 1 d . . . . .
H9 H 0.1909 0.8559 -0.0446 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3188(6) 0.7117(5) 0.0873(3) 0.0372(9) Uani 1 1 d . . . . .
H10 H 0.1840 0.7049 0.1221 0.045 Uiso 1 1 calc R U . . .
H2 H 0.947(5) 0.676(3) 0.737(2) 0.034(10) Uiso 1 1 d D . . . .
H1 H 0.792(4) 0.626(4) 0.705(3) 0.055(13) Uiso 1 1 d D . . . .
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'
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'
Cu Cu 0.3201 1.2651 '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
N1 Cu1 N2 93.73(10) . 2_766 ?
N1 Cu1 O3 171.20(9) . 2_766 ?
N2 Cu1 O3 80.05(9) 2_766 2_766 ?
N1 Cu1 O1 79.68(9) . . ?
N2 Cu1 O1 170.65(9) 2_766 . ?
O3 Cu1 O1 105.72(8) 2_766 . ?
N1 Cu1 O5 99.35(10) . . ?
N2 Cu1 O5 97.47(10) 2_766 . ?
O3 Cu1 O5 87.71(9) 2_766 . ?
O1 Cu1 O5 90.19(9) . . ?
C1 O1 Cu1 115.38(17) . . ?
C5 O3 Cu1 115.14(17) . 2_766 ?
Cu1 O5 H2 110(2) . . ?
Cu1 O5 H1 106(3) . . ?
H2 O5 H1 100.9(15) . . ?
N2 N1 C2 109.2(2) . . ?
N2 N1 Cu1 132.34(19) . . ?
C2 N1 Cu1 118.32(19) . . ?
N1 N2 C4 108.5(2) . . ?
N1 N2 Cu1 133.43(19) . 2_766 ?
C4 N2 Cu1 117.78(19) . 2_766 ?
C6 N3 C10 120.5(3) . . ?
C6 N3 H3 119.8 . . ?
C10 N3 H3 119.8 . . ?
C8 N4 H4A 120.0 . . ?
C8 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
O2 C1 O1 123.6(3) . . ?
O2 C1 C2 122.2(3) . . ?
O1 C1 C2 114.2(2) . . ?
N1 C2 C3 109.0(2) . . ?
N1 C2 C1 112.3(2) . . ?
C3 C2 C1 138.7(3) . . ?
C4 C3 C2 104.0(2) . . ?
C4 C3 H3A 128.0 . . ?
C2 C3 H3A 128.0 . . ?
N2 C4 C3 109.3(2) . . ?
N2 C4 C5 112.3(2) . . ?
C3 C4 C5 138.5(3) . . ?
O4 C5 O3 124.0(3) . . ?
O4 C5 C4 121.7(3) . . ?
O3 C5 C4 114.3(2) . . ?
N3 C6 C7 121.6(3) . . ?
N3 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 120.0(3) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
N4 C8 C9 121.7(3) . . ?
N4 C8 C7 121.8(3) . . ?
C9 C8 C7 116.6(3) . . ?
C10 C9 C8 119.9(3) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
N3 C10 C9 121.3(3) . . ?
N3 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
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
Cu1 N1 1.919(2) . ?
Cu1 N2 1.919(2) 2_766 ?
Cu1 O3 2.021(2) 2_766 ?
Cu1 O1 2.027(2) . ?
Cu1 O5 2.312(2) . ?
O1 C1 1.294(3) . ?
O2 C1 1.235(3) . ?
O3 C5 1.300(3) . ?
O3 Cu1 2.021(2) 2_766 ?
O4 C5 1.227(3) . ?
O5 H2 0.842(10) . ?
O5 H1 0.846(10) . ?
N1 N2 1.329(3) . ?
N1 C2 1.340(4) . ?
N2 C4 1.350(3) . ?
N2 Cu1 1.919(2) 2_766 ?
N3 C6 1.336(4) . ?
N3 C10 1.343(4) . ?
N3 H3 0.8600 . ?
N4 C8 1.320(4) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
C1 C2 1.490(4) . ?
C2 C3 1.399(4) . ?
C3 C4 1.390(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.487(4) . ?
C6 C7 1.347(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.418(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.412(4) . ?
C9 C10 1.354(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
