#------------------------------------------------------------------------------
#$Date: 2022-06-14 12:22:26 +0300 (Tue, 14 Jun 2022) $
#$Revision: 276023 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/54/8105412.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_8105412
loop_
_publ_author_name
'Qiao, Hong-Tao'
'Zhao, San-Hu'
'Xi, Fu-Gui'
_publ_section_title
;
 N′,N′′′-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(methaneylylidene))bis(2-hydroxybenzohydrazide)nickel(II),
 C30H24N4NiO6
;
_journal_issue                   5
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1171
_journal_page_last               1173
_journal_paper_doi               10.1515/ncrs-2020-0232
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C30 H24 N4 Ni O6'
_chemical_formula_sum            'C30 H24 N4 Ni O6'
_chemical_formula_weight         595.24
_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   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                100.7000(10)
_cell_angle_beta                 110.0900(10)
_cell_angle_gamma                104.7350(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5870(2)
_cell_length_b                   10.6944(2)
_cell_length_c                   13.6830(3)
_cell_measurement_reflns_used    8430
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.79
_cell_volume                     1342.02(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25704
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.111
_diffrn_reflns_theta_min         2.786
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0388
_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)+(0.0353P)²+0.5261P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4465
_reflns_number_total             5925
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2020-0232_suppl.cif
_cod_data_source_block           c30h24n4nio6
_cod_database_code               8105412
_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_max   0.867
_shelx_estimated_absorpt_t_min   0.824
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C27(H27), C28(H28),
  C29(H29), C30(H30)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
Ni1 Ni 0.65144(3) 0.40716(3) 0.26147(3) 0.03935(10) Uani 1 1 d . . . . .
O1 O 0.5282(2) 0.8661(2) 0.32221(16) 0.0810(7) Uani 1 1 d . . . . .
H1 H 0.510348 0.792199 0.280080 0.121 Uiso 1 1 calc GR . . . .
O2 O 0.75370(16) 0.59455(16) 0.36644(14) 0.0463(4) Uani 1 1 d . . . . .
O3 O 0.47137(16) 0.22311(16) 0.16405(14) 0.0473(4) Uani 1 1 d . . . . .
O4 O 0.57450(16) 0.35071(17) 0.38161(14) 0.0475(4) Uani 1 1 d . . . . .
O6 O 0.72072(16) 0.38333(16) 0.14241(14) 0.0455(4) Uani 1 1 d . . . . .
O7 O 1.04440(19) 0.2132(2) 0.19092(14) 0.0601(5) Uani 1 1 d . . . . .
H7 H 1.010064 0.235157 0.233919 0.090 Uiso 1 1 calc GR . . . .
N1 N 0.54941(19) 0.62983(18) 0.26290(15) 0.0397(4) Uani 1 1 d . . . . .
N2 N 0.51591(19) 0.49997(18) 0.19744(15) 0.0372(4) Uani 1 1 d . . . . .
N3 N 0.79987(19) 0.32613(18) 0.32299(16) 0.0391(4) Uani 1 1 d . . . . .
N4 N 0.8562(2) 0.28228(19) 0.25083(16) 0.0417(4) Uani 1 1 d . . . . .
C1 C 0.6399(3) 0.8877(2) 0.4163(2) 0.0498(6) Uani 1 1 d . . . . .
C2 C 0.7129(2) 0.7957(2) 0.43259(19) 0.0414(5) Uani 1 1 d . . . . .
C3 C 0.8235(3) 0.8268(3) 0.5340(2) 0.0628(8) Uani 1 1 d . . . . .
H3 H 0.871144 0.765573 0.547160 0.075 Uiso 1 1 calc R . . . .
C4 C 0.8656(3) 0.9446(3) 0.6157(2) 0.0749(9) Uani 1 1 d . . . . .
H4 H 0.939717 0.962515 0.683172 0.090 Uiso 1 1 calc R . . . .
C5 C 0.7958(4) 1.0355(3) 0.5959(2) 0.0700(9) Uani 1 1 d . . . . .
H5 H 0.825782 1.117425 0.649337 0.084 Uiso 1 1 calc R . . . .
C6 C 0.6838(3) 1.0069(3) 0.4992(2) 0.0650(8) Uani 1 1 d . . . . .
H6 H 0.635704 1.068109 0.488185 0.078 Uiso 1 1 calc R . . . .
C7 C 0.6719(2) 0.6657(2) 0.34979(19) 0.0390(5) Uani 1 1 d . . . . .
C8 C 0.4142(2) 0.4596(2) 0.1025(2) 0.0426(5) Uani 1 1 d . . . . .
H8 H 0.367808 0.519275 0.080946 0.051 Uiso 1 1 calc R . . . .
C9 C 0.3667(2) 0.3255(2) 0.0257(2) 0.0416(5) Uani 1 1 d . . . . .
C10 C 0.2876(3) 0.3071(3) -0.0842(2) 0.0512(6) Uani 1 1 d . . . . .
H10 H 0.264931 0.379232 -0.105203 0.061 Uiso 1 1 calc R . . . .
C11 C 0.2422(3) 0.1847(3) -0.1624(2) 0.0619(7) Uani 1 1 d . . . . .
H11 H 0.190675 0.175104 -0.235426 0.074 Uiso 1 1 calc R . . . .
C12 C 0.2736(3) 0.0767(3) -0.1320(3) 0.0693(8) Uani 1 1 d . . . . .
H12 H 0.243963 -0.005851 -0.184647 0.083 Uiso 1 1 calc R . . . .
C13 C 0.3493(3) 0.0911(3) -0.0229(3) 0.0627(8) Uani 1 1 d . . . . .
H13 H 0.369044 0.017672 -0.002346 0.075 Uiso 1 1 calc R . . . .
C14 C 0.3950(2) 0.2135(2) 0.0547(2) 0.0454(6) Uani 1 1 d . . . . .
C15 C 0.3800(3) 0.1940(3) 0.2214(2) 0.0643(8) Uani 1 1 d . . . . .
H15A H 0.312554 0.101867 0.187460 0.077 Uiso 1 1 calc R . . . .
H15B H 0.326532 0.255597 0.219678 0.077 Uiso 1 1 calc R . . . .
C16 C 0.4756(3) 0.2120(3) 0.3358(2) 0.0666(8) Uani 1 1 d . . . . .
H16A H 0.419418 0.194237 0.377920 0.080 Uiso 1 1 calc R . . . .
H16B H 0.527878 0.149466 0.337235 0.080 Uiso 1 1 calc R . . . .
C17 C 0.6764(2) 0.3773(2) 0.4877(2) 0.0452(6) Uani 1 1 d . . . . .
C18 C 0.6421(3) 0.4171(3) 0.5739(2) 0.0609(7) Uani 1 1 d . . . . .
H18 H 0.553389 0.426485 0.561002 0.073 Uiso 1 1 calc R . . . .
C19 C 0.7391(3) 0.4432(3) 0.6795(2) 0.0646(8) Uani 1 1 d . . . . .
H19 H 0.715809 0.471083 0.737571 0.078 Uiso 1 1 calc R . . . .
C20 C 0.8697(3) 0.4282(3) 0.6994(2) 0.0566(7) Uani 1 1 d . . . . .
H20 H 0.934552 0.445163 0.770581 0.068 Uiso 1 1 calc R . . . .
C21 C 0.9041(3) 0.3879(3) 0.6133(2) 0.0496(6) Uani 1 1 d . . . . .
H21 H 0.992672 0.377612 0.627217 0.060 Uiso 1 1 calc R . . . .
C22 C 0.8092(2) 0.3622(2) 0.5056(2) 0.0429(5) Uani 1 1 d . . . . .
C23 C 0.8559(3) 0.3209(3) 0.4203(2) 0.0471(6) Uani 1 1 d . . . . .
H23 H 0.931934 0.288559 0.437900 0.057 Uiso 1 1 calc R . . . .
C24 C 0.8047(2) 0.3146(2) 0.1595(2) 0.0394(5) Uani 1 1 d . . . . .
C25 C 0.8485(2) 0.2647(2) 0.07244(19) 0.0400(5) Uani 1 1 d . . . . .
C26 C 0.9642(2) 0.2174(2) 0.0917(2) 0.0434(5) Uani 1 1 d . . . . .
C27 C 0.9992(3) 0.1726(3) 0.0062(2) 0.0549(7) Uani 1 1 d . . . . .
H27 H 1.077156 0.143008 0.019340 0.066 Uiso 1 1 calc R . . . .
C28 C 0.9211(3) 0.1712(3) -0.0970(2) 0.0640(8) Uani 1 1 d . . . . .
H28 H 0.946788 0.141396 -0.153280 0.077 Uiso 1 1 calc R . . . .
C29 C 0.8039(3) 0.2136(3) -0.1189(2) 0.0653(8) Uani 1 1 d . . . . .
H29 H 0.749550 0.210777 -0.189563 0.078 Uiso 1 1 calc R . . . .
C30 C 0.7692(3) 0.2602(3) -0.0342(2) 0.0535(6) Uani 1 1 d . . . . .
H30 H 0.690884 0.289334 -0.048418 0.064 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'
Ni Ni 0.3393 1.1124 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Ni1 O3 156.14(6) . .
O2 Ni1 O4 87.50(7) . .
O2 Ni1 O6 111.05(7) . .
O3 Ni1 O4 77.70(6) . .
O6 Ni1 O3 88.29(7) . .
O6 Ni1 O4 157.24(6) . .
N2 Ni1 O2 79.49(7) . .
N2 Ni1 O3 84.58(7) . .
N2 Ni1 O4 99.52(7) . .
N2 Ni1 O6 96.87(7) . .
N3 Ni1 O2 98.04(7) . .
N3 Ni1 O3 99.11(7) . .
N3 Ni1 O4 84.79(7) . .
N3 Ni1 O6 79.77(7) . .
N3 Ni1 N2 174.88(7) . .
C7 O2 Ni1 110.17(14) . .
C14 O3 Ni1 116.70(13) . .
C14 O3 C15 113.08(18) . .
C15 O3 Ni1 109.71(15) . .
C16 O4 Ni1 109.32(15) . .
C17 O4 Ni1 117.91(13) . .
C17 O4 C16 112.90(18) . .
C24 O6 Ni1 110.04(14) . .
C7 N1 N2 110.70(17) . .
N1 N2 Ni1 113.61(13) . .
C8 N2 Ni1 128.11(15) . .
C8 N2 N1 117.93(18) . .
N4 N3 Ni1 113.55(14) . .
C23 N3 Ni1 128.53(15) . .
C23 N3 N4 117.61(18) . .
C24 N4 N3 110.77(17) . .
O1 C1 C2 122.6(2) . .
O1 C1 C6 117.9(2) . .
C6 C1 C2 119.5(2) . .
C1 C2 C7 123.1(2) . .
C3 C2 C1 117.4(2) . .
C3 C2 C7 119.3(2) . .
C4 C3 C2 122.5(2) . .
C3 C4 C5 118.7(3) . .
C6 C5 C4 120.7(3) . .
C5 C6 C1 121.0(3) . .
O2 C7 N1 124.5(2) . .
O2 C7 C2 118.9(2) . .
N1 C7 C2 116.51(19) . .
N2 C8 C9 123.8(2) . .
C10 C9 C8 117.9(2) . .
C10 C9 C14 117.6(2) . .
C14 C9 C8 124.5(2) . .
C11 C10 C9 121.6(3) . .
C10 C11 C12 119.7(3) . .
C11 C12 C13 120.0(3) . .
C14 C13 C12 120.1(3) . .
C9 C14 O3 121.0(2) . .
C13 C14 O3 118.0(2) . .
C13 C14 C9 121.0(3) . .
O3 C15 C16 106.9(2) . .
O4 C16 C15 107.8(2) . .
C18 C17 O4 118.4(2) . .
C18 C17 C22 120.7(2) . .
C22 C17 O4 120.9(2) . .
C17 C18 C19 120.2(2) . .
C20 C19 C18 120.4(3) . .
C19 C20 C21 119.6(3) . .
C20 C21 C22 121.5(2) . .
C17 C22 C23 125.0(2) . .
C21 C22 C17 117.6(2) . .
C21 C22 C23 117.4(2) . .
N3 C23 C22 124.6(2) . .
O6 C24 N4 124.9(2) . .
O6 C24 C25 119.0(2) . .
N4 C24 C25 116.10(18) . .
C26 C25 C24 122.8(2) . .
C30 C25 C24 119.0(2) . .
C30 C25 C26 118.2(2) . .
O7 C26 C25 122.8(2) . .
O7 C26 C27 117.6(2) . .
C27 C26 C25 119.6(2) . .
C28 C27 C26 120.9(2) . .
C27 C28 C29 120.7(3) . .
C30 C29 C28 118.9(3) . .
C29 C30 C25 121.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.0026(16) .
Ni1 O3 2.1580(16) .
Ni1 O4 2.1836(16) .
Ni1 O6 2.0047(16) .
Ni1 N2 1.9988(18) .
Ni1 N3 1.9960(18) .
O1 C1 1.347(3) .
O2 C7 1.283(2) .
O3 C14 1.405(3) .
O3 C15 1.451(3) .
O4 C16 1.450(3) .
O4 C17 1.403(3) .
O6 C24 1.280(2) .
O7 C26 1.348(3) .
N1 N2 1.388(2) .
N1 C7 1.327(3) .
N2 C8 1.276(3) .
N3 N4 1.388(2) .
N3 C23 1.276(3) .
N4 C24 1.329(3) .
C1 C2 1.402(3) .
C1 C6 1.387(3) .
C2 C3 1.386(3) .
C2 C7 1.475(3) .
C3 C4 1.373(4) .
C4 C5 1.374(4) .
C5 C6 1.356(4) .
C8 C9 1.458(3) .
C9 C10 1.394(3) .
C9 C14 1.399(3) .
C10 C11 1.377(4) .
C11 C12 1.377(4) .
C12 C13 1.388(4) .
C13 C14 1.373(3) .
C15 C16 1.487(4) .
C17 C18 1.375(3) .
C17 C22 1.399(3) .
C18 C19 1.381(4) .
C19 C20 1.372(4) .
C20 C21 1.375(3) .
C21 C22 1.396(3) .
C22 C23 1.455(3) .
C24 C25 1.479(3) .
C25 C26 1.403(3) .
C25 C30 1.396(3) .
C26 C27 1.384(3) .
C27 C28 1.366(4) .
C28 C29 1.384(4) .
C29 C30 1.378(4) .
