#------------------------------------------------------------------------------
#$Date: 2025-08-21 22:04:39 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301851 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/26/7052615.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_7052615
loop_
_publ_author_name
'Gong, Yunnan'
'Liu, Chongbo'
'Wen, Huiliang'
'Yan, Liushui'
'Xiong, Zhiqiang'
'Ding, Liang'
_publ_section_title
;
 Structural diversity and properties of M(ii) phenyl substituted
 pyrazole carboxylate complexes with 0D-, 1D-, 2D- and 3D frameworks
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              865
_journal_paper_doi               10.1039/c0nj00904k
_journal_volume                  35
_journal_year                    2011
_chemical_formula_sum            'C20 H18 N4 Ni O6'
_chemical_formula_weight         469.09
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.406(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.8445(9)
_cell_length_b                   32.906(6)
_cell_length_c                   6.2836(11)
_cell_measurement_reflns_used    2058
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.48
_cell_volume                     965.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8567
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.8421
_exptl_absorpt_correction_T_min  0.7114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0552P)²+0.7610P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                1725
_reflns_number_total             2212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00904k.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7052615
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.0000 0.02559(6) Uani 1 2 d S . .
O1 O 0.3363(2) 0.01825(3) 0.25732(15) 0.0285(2) Uani 1 1 d . . .
O2 O 0.3464(2) 0.06954(3) 0.49311(16) 0.0373(3) Uani 1 1 d . . .
O3 O 0.1419(2) 0.02783(3) -0.22653(15) 0.0293(3) Uani 1 1 d . . .
H1W H 0.1949 0.0362 -0.3315 0.044 Uiso 1 1 d R . .
H2W H 0.0157 0.0108 -0.2674 0.044 Uiso 1 1 d R . .
N1 N 0.6803(2) 0.05523(4) 0.06525(18) 0.0273(3) Uani 1 1 d . . .
N2 N 0.8382(2) 0.08082(4) -0.01858(19) 0.0292(3) Uani 1 1 d . . .
H2 H 0.9149 0.0746 -0.1230 0.035 Uiso 1 1 calc R . .
C1 C 0.4131(3) 0.05338(4) 0.3355(2) 0.0263(4) Uani 1 1 d . . .
C2 C 0.6006(3) 0.07620(4) 0.2209(2) 0.0256(3) Uani 1 1 d . . .
C3 C 0.7089(3) 0.11535(5) 0.2370(2) 0.0298(4) Uani 1 1 d . . .
H3 H 0.6837 0.1358 0.3324 0.036 Uiso 1 1 calc R . .
C4 C 0.8631(3) 0.11758(4) 0.0800(2) 0.0276(4) Uani 1 1 d . . .
C5 C 1.0280(3) 0.15063(5) 0.0160(3) 0.0334(4) Uani 1 1 d . . .
C6 C 1.0842(4) 0.18559(5) 0.1394(3) 0.0515(6) Uani 1 1 d . . .
H6 H 1.0113 0.1885 0.2613 0.062 Uiso 1 1 calc R . .
C7 C 1.2475(5) 0.21654(6) 0.0856(4) 0.0704(7) Uani 1 1 d . . .
H7 H 1.2867 0.2398 0.1725 0.085 Uiso 1 1 calc R . .
C8 C 1.3503(5) 0.21275(6) -0.0954(4) 0.0740(7) Uani 1 1 d . . .
H8 H 1.4595 0.2335 -0.1323 0.089 Uiso 1 1 calc R . .
C9 C 1.2934(4) 0.17856(6) -0.2226(3) 0.0606(6) Uani 1 1 d . . .
H9 H 1.3634 0.1764 -0.3463 0.073 Uiso 1 1 calc R . .
C10 C 1.1338(4) 0.14720(6) -0.1706(3) 0.0453(5) Uani 1 1 d . . .
H10 H 1.0967 0.1240 -0.2583 0.054 Uiso 1 1 calc R . .
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'
Ni Ni 0.3393 1.1124 '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 Ni1 N1 180.00(3) . 3_655 ?
N1 Ni1 O1 79.30(5) . . ?
N1 Ni1 O1 100.70(5) 3_655 . ?
N1 Ni1 O1 100.70(5) . 3_655 ?
N1 Ni1 O1 79.30(5) 3_655 3_655 ?
O1 Ni1 O1 180.00(7) . 3_655 ?
N1 Ni1 O3 91.13(4) . 3_655 ?
N1 Ni1 O3 88.87(4) 3_655 3_655 ?
O1 Ni1 O3 90.90(4) . 3_655 ?
O1 Ni1 O3 89.10(4) 3_655 3_655 ?
N1 Ni1 O3 88.87(4) . . ?
N1 Ni1 O3 91.13(4) 3_655 . ?
O1 Ni1 O3 89.10(4) . . ?
O1 Ni1 O3 90.90(4) 3_655 . ?
O3 Ni1 O3 180.00(5) 3_655 . ?
C1 O1 Ni1 115.57(9) . . ?
Ni1 O3 H1W 108.0 . . ?
Ni1 O3 H2W 108.8 . . ?
H1W O3 H2W 110.2 . . ?
C2 N1 N2 105.68(12) . . ?
C2 N1 Ni1 114.97(10) . . ?
N2 N1 Ni1 138.78(10) . . ?
N1 N2 C4 111.99(13) . . ?
N1 N2 H2 124.0 . . ?
C4 N2 H2 124.0 . . ?
O2 C1 O1 125.89(14) . . ?
O2 C1 C2 119.19(13) . . ?
O1 C1 C2 114.92(12) . . ?
N1 C2 C3 110.91(13) . . ?
N1 C2 C1 114.98(12) . . ?
C3 C2 C1 134.10(14) . . ?
C2 C3 C4 105.20(13) . . ?
C2 C3 H3 127.4 . . ?
C4 C3 H3 127.4 . . ?
N2 C4 C3 106.23(13) . . ?
N2 C4 C5 121.81(14) . . ?
C3 C4 C5 131.96(14) . . ?
C6 C5 C10 118.51(17) . . ?
C6 C5 C4 120.46(16) . . ?
C10 C5 C4 121.03(15) . . ?
C5 C6 C7 121.2(2) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 119.7(2) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 120.1(2) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C8 C9 C10 121.1(2) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C9 C10 C5 119.33(18) . . ?
C9 C10 H10 120.3 . . ?
C5 C10 H10 120.3 . . ?
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
Ni1 N1 2.0110(12) . ?
Ni1 N1 2.0110(12) 3_655 ?
Ni1 O1 2.0702(11) . ?
Ni1 O1 2.0702(11) 3_655 ?
Ni1 O3 2.1359(9) 3_655 ?
Ni1 O3 2.1359(9) . ?
O1 C1 1.2723(17) . ?
O2 C1 1.2403(18) . ?
O3 H1W 0.8165 . ?
O3 H2W 0.8189 . ?
N1 C2 1.3348(19) . ?
N1 N2 1.3363(18) . ?
N2 C4 1.3498(19) . ?
N2 H2 0.8600 . ?
C1 C2 1.502(2) . ?
C2 C3 1.385(2) . ?
C3 C4 1.388(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.467(2) . ?
C5 C6 1.373(2) . ?
C5 C10 1.403(3) . ?
C6 C7 1.385(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.363(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.365(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.380(3) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H2W O1 0.82 1.97 2.7323(14) 154.5 3
O3 H1W O2 0.82 1.84 2.6261(15) 161.0 1_554
N2 H2 O3 0.86 2.09 2.8169(17) 141.4 1_655
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 O1 C1 0.48(9) . . . . ?
N1 Ni1 O1 C1 -179.52(9) 3_655 . . . ?
O1 Ni1 O1 C1 -104.00(14) 3_655 . . . ?
O3 Ni1 O1 C1 91.46(9) 3_655 . . . ?
O3 Ni1 O1 C1 -88.54(9) . . . . ?
N1 Ni1 N1 C2 143(100) 3_655 . . . ?
O1 Ni1 N1 C2 -3.52(9) . . . . ?
O1 Ni1 N1 C2 176.48(9) 3_655 . . . ?
O3 Ni1 N1 C2 -94.23(9) 3_655 . . . ?
O3 Ni1 N1 C2 85.77(9) . . . . ?
N1 Ni1 N1 N2 -26(100) 3_655 . . . ?
O1 Ni1 N1 N2 -173.26(14) . . . . ?
O1 Ni1 N1 N2 6.74(14) 3_655 . . . ?
O3 Ni1 N1 N2 96.04(13) 3_655 . . . ?
O3 Ni1 N1 N2 -83.96(13) . . . . ?
C2 N1 N2 C4 0.33(14) . . . . ?
Ni1 N1 N2 C4 170.67(10) . . . . ?
Ni1 O1 C1 O2 -177.82(11) . . . . ?
Ni1 O1 C1 C2 2.32(14) . . . . ?
N2 N1 C2 C3 -0.17(14) . . . . ?
Ni1 N1 C2 C3 -173.17(9) . . . . ?
N2 N1 C2 C1 178.71(10) . . . . ?
Ni1 N1 C2 C1 5.71(14) . . . . ?
O2 C1 C2 N1 174.78(12) . . . . ?
O1 C1 C2 N1 -5.35(16) . . . . ?
O2 C1 C2 C3 -6.7(2) . . . . ?
O1 C1 C2 C3 173.19(14) . . . . ?
N1 C2 C3 C4 -0.03(15) . . . . ?
C1 C2 C3 C4 -178.62(13) . . . . ?
N1 N2 C4 C3 -0.35(15) . . . . ?
N1 N2 C4 C5 179.74(11) . . . . ?
C2 C3 C4 N2 0.22(14) . . . . ?
C2 C3 C4 C5 -179.88(14) . . . . ?
N2 C4 C5 C6 -170.59(14) . . . . ?
C3 C4 C5 C6 9.5(2) . . . . ?
N2 C4 C5 C10 8.9(2) . . . . ?
C3 C4 C5 C10 -171.03(15) . . . . ?
C10 C5 C6 C7 -1.6(3) . . . . ?
C4 C5 C6 C7 177.86(16) . . . . ?
C5 C6 C7 C8 1.3(3) . . . . ?
C6 C7 C8 C9 -0.2(3) . . . . ?
C7 C8 C9 C10 -0.5(3) . . . . ?
C8 C9 C10 C5 0.1(3) . . . . ?
C6 C5 C10 C9 0.9(2) . . . . ?
C4 C5 C10 C9 -178.55(15) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168349082
