#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:27:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180080 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/26/7052618.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_7052618
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
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.7360(10)
_cell_angle_beta                 82.9990(10)
_cell_angle_gamma                75.0920(10)
_cell_formula_units_Z            1
_cell_length_a                   6.6139(7)
_cell_length_b                   6.9872(7)
_cell_length_c                   10.4414(11)
_cell_measurement_reflns_used    1808
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      3.38
_cell_volume                     457.35(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3527
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             242
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0292
_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)+(0.0303P)²+0.2683P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0689
_reflns_number_gt                1548
_reflns_number_total             1683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00904k.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               7052618
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.5000 0.01709(13) Uani 1 2 d S . .
O1 O 0.3139(3) 0.8312(2) 0.44969(16) 0.0297(4) Uani 1 1 d . . .
O2 O 0.0696(2) 0.9497(2) 0.30675(15) 0.0248(4) Uani 1 1 d . . .
O3 O 0.6455(2) 0.0138(2) 0.30931(15) 0.0289(4) Uani 1 1 d . . .
H1W H 0.7728 -0.0072 0.3122 0.043 Uiso 1 1 d R . .
H2W H 0.6113 -0.0846 0.2742 0.043 Uiso 1 1 d R . .
N1 N 0.2812(3) 0.2630(3) 0.44194(17) 0.0189(4) Uani 1 1 d . . .
N2 N 0.1528(3) 0.3029(3) 0.34414(16) 0.0192(4) Uani 1 1 d . . .
H2 H 0.1171 0.2125 0.3119 0.023 Uiso 1 1 calc R . .
C1 C 0.2940(3) 0.4400(3) 0.4634(2) 0.0175(4) Uani 1 1 d . . .
H1 H 0.3697 0.4580 0.5279 0.021 Uiso 1 1 calc R . .
C2 C 0.1808(3) 0.5968(3) 0.37821(19) 0.0166(4) Uani 1 1 d . . .
C3 C 0.0875(3) 0.5017(3) 0.3032(2) 0.0173(4) Uani 1 1 d . . .
C4 C 0.1849(3) 0.8095(3) 0.3774(2) 0.0180(4) Uani 1 1 d . . .
C5 C -0.0626(3) 0.5775(3) 0.2011(2) 0.0200(5) Uani 1 1 d . . .
C6 C -0.0292(4) 0.7220(3) 0.0968(2) 0.0274(5) Uani 1 1 d . . .
H6 H 0.0916 0.7693 0.0886 0.033 Uiso 1 1 calc R . .
C7 C -0.1744(5) 0.7960(4) 0.0048(2) 0.0394(7) Uani 1 1 d . . .
H7 H -0.1496 0.8914 -0.0656 0.047 Uiso 1 1 calc R . .
C8 C -0.3545(5) 0.7300(4) 0.0164(3) 0.0436(7) Uani 1 1 d . . .
H8 H -0.4536 0.7835 -0.0445 0.052 Uiso 1 1 calc R . .
C9 C -0.3889(4) 0.5834(4) 0.1190(3) 0.0385(6) Uani 1 1 d . . .
H9 H -0.5104 0.5372 0.1265 0.046 Uiso 1 1 calc R . .
C10 C -0.2419(4) 0.5055(4) 0.2105(2) 0.0271(5) Uani 1 1 d . . .
H10 H -0.2635 0.4049 0.2783 0.033 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 180.0 . 2_656 ?
N1 Ni1 O1 90.97(6) . 1_545 ?
N1 Ni1 O1 89.03(6) 2_656 1_545 ?
N1 Ni1 O1 89.03(6) . 2_666 ?
N1 Ni1 O1 90.97(6) 2_656 2_666 ?
O1 Ni1 O1 180.00(5) 1_545 2_666 ?
N1 Ni1 O3 90.38(7) . 2_656 ?
N1 Ni1 O3 89.62(7) 2_656 2_656 ?
O1 Ni1 O3 90.93(7) 1_545 2_656 ?
O1 Ni1 O3 89.07(7) 2_666 2_656 ?
N1 Ni1 O3 89.62(7) . . ?
N1 Ni1 O3 90.38(7) 2_656 . ?
O1 Ni1 O3 89.07(7) 1_545 . ?
O1 Ni1 O3 90.93(7) 2_666 . ?
O3 Ni1 O3 180.0 2_656 . ?
C4 O1 Ni1 150.44(14) . 1_565 ?
Ni1 O3 H1W 109.4 . . ?
Ni1 O3 H2W 105.6 . . ?
H1W O3 H2W 111.2 . . ?
C1 N1 N2 105.20(16) . . ?
C1 N1 Ni1 122.98(14) . . ?
N2 N1 Ni1 128.20(13) . . ?
C3 N2 N1 111.82(16) . . ?
C3 N2 H2 124.1 . . ?
N1 N2 H2 124.1 . . ?
N1 C1 C2 112.21(18) . . ?
N1 C1 H1 123.9 . . ?
C2 C1 H1 123.9 . . ?
C1 C2 C3 104.12(17) . . ?
C1 C2 C4 121.85(18) . . ?
C3 C2 C4 133.97(18) . . ?
N2 C3 C2 106.60(17) . . ?
N2 C3 C5 120.38(18) . . ?
C2 C3 C5 132.96(18) . . ?
O2 C4 O1 125.04(19) . . ?
O2 C4 C2 120.73(18) . . ?
O1 C4 C2 114.21(17) . . ?
C6 C5 C10 119.2(2) . . ?
C6 C5 C3 121.1(2) . . ?
C10 C5 C3 119.74(19) . . ?
C7 C6 C5 120.3(2) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C6 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 119.9(2) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C8 C9 C10 119.9(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C5 120.1(2) . . ?
C9 C10 H10 119.9 . . ?
C5 C10 H10 119.9 . . ?
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 2.0706(17) . ?
Ni1 N1 2.0706(17) 2_656 ?
Ni1 O1 2.0755(14) 1_545 ?
Ni1 O1 2.0755(14) 2_666 ?
Ni1 O3 2.1005(15) 2_656 ?
Ni1 O3 2.1005(15) . ?
O1 C4 1.259(2) . ?
O1 Ni1 2.0755(14) 1_565 ?
O2 C4 1.257(2) . ?
O3 H1W 0.8200 . ?
O3 H2W 0.9213 . ?
N1 C1 1.320(3) . ?
N1 N2 1.353(2) . ?
N2 C3 1.351(3) . ?
N2 H2 0.8600 . ?
C1 C2 1.395(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.396(3) . ?
C2 C4 1.492(3) . ?
C3 C5 1.479(3) . ?
C5 C6 1.385(3) . ?
C5 C10 1.390(3) . ?
C6 C7 1.379(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.369(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.385(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.387(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 H1W O2 0.82 1.90 2.721(2) 176.2 1_645
N2 H2 O2 0.86 1.95 2.764(2) 157.0 1_545
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 N1 C1 -76(100) 2_656 . . . ?
O1 Ni1 N1 C1 171.64(17) 1_545 . . . ?
O1 Ni1 N1 C1 -8.36(17) 2_666 . . . ?
O3 Ni1 N1 C1 80.70(17) 2_656 . . . ?
O3 Ni1 N1 C1 -99.30(17) . . . . ?
N1 Ni1 N1 N2 79(100) 2_656 . . . ?
O1 Ni1 N1 N2 -33.07(17) 1_545 . . . ?
O1 Ni1 N1 N2 146.93(17) 2_666 . . . ?
O3 Ni1 N1 N2 -124.01(17) 2_656 . . . ?
O3 Ni1 N1 N2 55.99(17) . . . . ?
C1 N1 N2 C3 0.8(2) . . . . ?
Ni1 N1 N2 C3 -157.92(15) . . . . ?
N2 N1 C1 C2 -1.9(2) . . . . ?
Ni1 N1 C1 C2 158.22(14) . . . . ?
N1 C1 C2 C3 2.2(2) . . . . ?
N1 C1 C2 C4 -175.39(19) . . . . ?
N1 N2 C3 C2 0.6(2) . . . . ?
N1 N2 C3 C5 -177.01(18) . . . . ?
C1 C2 C3 N2 -1.6(2) . . . . ?
C4 C2 C3 N2 175.6(2) . . . . ?
C1 C2 C3 C5 175.5(2) . . . . ?
C4 C2 C3 C5 -7.3(4) . . . . ?
Ni1 O1 C4 O2 -20.3(5) 1_565 . . . ?
Ni1 O1 C4 C2 158.3(2) 1_565 . . . ?
C1 C2 C4 O2 -174.6(2) . . . . ?
C3 C2 C4 O2 8.6(4) . . . . ?
C1 C2 C4 O1 6.8(3) . . . . ?
C3 C2 C4 O1 -170.0(2) . . . . ?
N2 C3 C5 C6 -133.4(2) . . . . ?
C2 C3 C5 C6 49.7(3) . . . . ?
N2 C3 C5 C10 47.6(3) . . . . ?
C2 C3 C5 C10 -129.3(3) . . . . ?
C10 C5 C6 C7 1.2(3) . . . . ?
C3 C5 C6 C7 -177.8(2) . . . . ?
C5 C6 C7 C8 1.0(4) . . . . ?
C6 C7 C8 C9 -2.0(4) . . . . ?
C7 C8 C9 C10 0.7(4) . . . . ?
C8 C9 C10 C5 1.5(4) . . . . ?
C6 C5 C10 C9 -2.4(3) . . . . ?
C3 C5 C10 C9 176.6(2) . . . . ?
