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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/7/06/24/7062431.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_7062431
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            'C14 H22 Cu3 N8 O10'
_chemical_formula_weight         653.01
_chemical_name_common
{diaqua-bis(ethylenediamine)-bis(mu-pyrazole-3,5-dicarbarboxylato)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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-11-14 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                114.0320(10)
_cell_angle_beta                 94.7760(10)
_cell_angle_gamma                101.9570(10)
_cell_formula_units_Z            1
_cell_length_a                   7.1285(2)
_cell_length_b                   8.7861(3)
_cell_length_c                   9.7390(4)
_cell_measurement_reflns_used    4342.5
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.375
_cell_measurement_theta_min      2.974
_cell_volume                     535.33(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0729
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18542
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         2.974
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.026
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_description       block
_exptl_crystal_F_000             329
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0313
_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)+(0.0294P)²+0.5553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2085
_reflns_number_total             2456
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj00821e2.cif
_cod_data_source_block           compound7
_cod_depositor_comments
'Adding full bibliography for 7062429--7062435.cif.'
_cod_database_code               7062431
_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   0.518
_shelx_estimated_absorpt_t_max   0.713
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 0.77847(4) 0.45968(4) 0.70682(3) 0.01698(11) Uani 1 1 d . . . . .
Cu2 Cu 1.0000 0.0000 0.5000 0.01932(13) Uani 1 2 d S . P . .
O1 O 0.4972(3) 0.4421(2) 0.6507(2) 0.0240(4) Uani 1 1 d . . . . .
O2 O 0.2298(3) 0.2699(3) 0.4751(2) 0.0242(4) Uani 1 1 d . . . . .
O3 O 0.9117(3) -0.1534(2) 0.2774(2) 0.0229(4) Uani 1 1 d . . . . .
O4 O 0.6516(3) -0.2450(2) 0.0914(2) 0.0250(4) Uani 1 1 d . . . . .
O5 O 0.7310(3) 0.4395(3) 0.9326(2) 0.0261(4) Uani 1 1 d . . . . .
N1 N 0.7030(3) 0.2212(3) 0.5417(2) 0.0154(4) Uani 1 1 d . . . . .
N2 N 0.7906(3) 0.1004(3) 0.4625(2) 0.0159(4) Uani 1 1 d . . . . .
N3 N 0.8441(4) 0.7187(3) 0.8181(3) 0.0226(5) Uani 1 1 d . . . . .
N4 N 1.0649(3) 0.4932(3) 0.7408(3) 0.0216(5) Uani 1 1 d . . . . .
C1 C 0.4058(4) 0.3075(3) 0.5310(3) 0.0176(5) Uani 1 1 d . . . . .
C2 C 0.5261(3) 0.1865(3) 0.4576(3) 0.0155(5) Uani 1 1 d . . . . .
C3 C 0.4967(4) 0.0421(3) 0.3203(3) 0.0191(5) Uani 1 1 d . . . . .
H3 H 0.3882 -0.0094 0.2416 0.023 Uiso 1 1 calc R U . . .
C4 C 0.6685(4) -0.0080(3) 0.3282(3) 0.0164(5) Uani 1 1 d . . . . .
C5 C 0.7458(4) -0.1466(3) 0.2237(3) 0.0187(5) Uani 1 1 d . . . . .
C6 C 1.0524(4) 0.7854(3) 0.8921(3) 0.0272(6) Uani 1 1 d . . . . .
H6A H 1.0690 0.7788 0.9892 0.033 Uiso 1 1 calc R U . . .
H6B H 1.1001 0.9053 0.9111 0.033 Uiso 1 1 calc R U . . .
C7 C 1.1645(4) 0.6760(4) 0.7856(4) 0.0283(6) Uani 1 1 d . . . . .
H7A H 1.1669 0.6979 0.6957 0.034 Uiso 1 1 calc R U . . .
H7B H 1.2980 0.7034 0.8369 0.034 Uiso 1 1 calc R U . . .
H1 H 0.716(5) 0.528(5) 0.989(4) 0.029(9) Uiso 1 1 d . . . . .
H2 H 0.638(6) 0.371(6) 0.927(5) 0.053(13) Uiso 1 1 d . . . . .
H3A H 0.830(5) 0.752(5) 0.757(4) 0.033(10) Uiso 1 1 d . . . . .
H3B H 0.773(5) 0.755(5) 0.881(4) 0.037(10) Uiso 1 1 d . . . . .
H4A H 1.108(5) 0.431(5) 0.673(4) 0.031(9) Uiso 1 1 d . . . . .
H4B H 1.095(5) 0.467(5) 0.814(4) 0.034(10) Uiso 1 1 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 N4 98.29(9) . . ?
N1 Cu1 O1 82.22(8) . . ?
N4 Cu1 O1 171.28(10) . . ?
N1 Cu1 N3 162.04(10) . . ?
N4 Cu1 N3 84.82(10) . . ?
O1 Cu1 N3 92.08(9) . . ?
N1 Cu1 O5 106.89(9) . . ?
N4 Cu1 O5 96.54(10) . . ?
O1 Cu1 O5 91.61(8) . . ?
N3 Cu1 O5 90.21(10) . . ?
N2 Cu2 N2 180.0 . 2_756 ?
N2 Cu2 O3 82.21(8) . . ?
N2 Cu2 O3 97.79(8) 2_756 . ?
N2 Cu2 O3 97.79(8) . 2_756 ?
N2 Cu2 O3 82.21(8) 2_756 2_756 ?
O3 Cu2 O3 180.0 . 2_756 ?
C1 O1 Cu1 114.61(15) . . ?
C5 O3 Cu2 113.23(16) . . ?
Cu1 O5 H1 107(3) . . ?
Cu1 O5 H2 116(3) . . ?
H1 O5 H2 104(4) . . ?
N2 N1 C2 107.96(19) . . ?
N2 N1 Cu1 138.20(16) . . ?
C2 N1 Cu1 110.82(15) . . ?
N1 N2 C4 107.85(19) . . ?
N1 N2 Cu2 138.95(16) . . ?
C4 N2 Cu2 110.74(16) . . ?
C6 N3 Cu1 108.95(17) . . ?
C6 N3 H3A 108(3) . . ?
Cu1 N3 H3A 107(3) . . ?
C6 N3 H3B 111(2) . . ?
Cu1 N3 H3B 114(3) . . ?
H3A N3 H3B 108(4) . . ?
C7 N4 Cu1 109.63(17) . . ?
C7 N4 H4A 110(2) . . ?
Cu1 N4 H4A 117(2) . . ?
C7 N4 H4B 110(2) . . ?
Cu1 N4 H4B 107(2) . . ?
H4A N4 H4B 102(3) . . ?
O2 C1 O1 125.6(2) . . ?
O2 C1 C2 119.7(2) . . ?
O1 C1 C2 114.7(2) . . ?
N1 C2 C3 110.7(2) . . ?
N1 C2 C1 115.1(2) . . ?
C3 C2 C1 134.2(2) . . ?
C2 C3 C4 103.3(2) . . ?
C2 C3 H3 128.4 . . ?
C4 C3 H3 128.4 . . ?
N2 C4 C3 110.2(2) . . ?
N2 C4 C5 115.0(2) . . ?
C3 C4 C5 134.7(2) . . ?
O4 C5 O3 124.5(2) . . ?
O4 C5 C4 120.1(2) . . ?
O3 C5 C4 115.3(2) . . ?
N3 C6 C7 107.8(2) . . ?
N3 C6 H6A 110.1 . . ?
C7 C6 H6A 110.1 . . ?
N3 C6 H6B 110.1 . . ?
C7 C6 H6B 110.1 . . ?
H6A C6 H6B 108.5 . . ?
N4 C7 C6 107.5(2) . . ?
N4 C7 H7A 110.2 . . ?
C6 C7 H7A 110.2 . . ?
N4 C7 H7B 110.2 . . ?
C6 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
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 1.977(2) . ?
Cu1 N4 1.981(2) . ?
Cu1 O1 1.9907(18) . ?
Cu1 N3 2.009(2) . ?
Cu1 O5 2.324(2) . ?
Cu2 N2 1.964(2) . ?
Cu2 N2 1.964(2) 2_756 ?
Cu2 O3 1.9883(18) . ?
Cu2 O3 1.9884(18) 2_756 ?
O1 C1 1.270(3) . ?
O2 C1 1.244(3) . ?
O3 C5 1.276(3) . ?
O4 C5 1.251(3) . ?
O5 H1 0.78(4) . ?
O5 H2 0.78(5) . ?
N1 N2 1.341(3) . ?
N1 C2 1.349(3) . ?
N2 C4 1.352(3) . ?
N3 C6 1.478(4) . ?
N3 H3A 0.77(4) . ?
N3 H3B 0.83(4) . ?
N4 C7 1.476(4) . ?
N4 H4A 0.80(4) . ?
N4 H4B 0.85(4) . ?
C1 C2 1.495(3) . ?
C2 C3 1.379(4) . ?
C3 C4 1.391(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.478(3) . ?
C6 C7 1.511(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
