#------------------------------------------------------------------------------
#$Date: 2019-11-23 18:51:03 +0100 (Sat 23 de Nov de 2019) $
#$Revision: 234724 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/20/7702062.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_7702062
loop_
_publ_author_name
'Jiang, Lin'
'Zhang, Dong-Yan'
'Suo, Jing-Jing'
'Gu, Wen'
'Tian, Jin-Lei'
'Liu, Xin'
'Yan, Shi-Ping'
_publ_section_title
;
 Synthesis, magnetism and spectral studies of six defective dicubane
 tetranuclear {M4O6} (M = Ni(II), Co(II), Zn(II)) and three trinuclear
 Cd(II) complexes with polydentate Schiff base ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10233
_journal_page_last               10248
_journal_paper_doi               10.1039/c6dt00380j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C46 H60 Cl6 N4 Ni4 O16'
_chemical_formula_weight         1372.52
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_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
_audit_update_record
;
2015-06-23 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4859(19)
_cell_length_b                   19.986(4)
_cell_length_c                   14.498(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2727.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27922
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.724
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_refine_diff_density_max         0.973
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1552P)²+6.7572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2506
_reflns_number_gt                3848
_reflns_number_total             4819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00380j2.cif
_cod_data_source_block           nini
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2727.3(9)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7702062
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
Ni2 Ni 0.52078(9) 0.12008(4) 0.41729(5) 0.0340(3) Uani 1 1 d .
N2 N 0.4272(6) 0.1625(3) 0.3021(4) 0.0388(13) Uani 1 1 d .
O1 O 0.7324(6) 0.1832(3) 0.4107(4) 0.0514(13) Uani 1 1 d .
O2 O 0.6663(5) 0.0897(2) 0.5198(3) 0.0339(10) Uani 1 1 d .
O4 O 0.4603(5) 0.1958(2) 0.4946(3) 0.0429(12) Uani 1 1 d .
O7 O 0.4020(4) 0.0511(2) 0.4803(3) 0.0322(10) Uani 1 1 d .
C21 C 0.2563(7) 0.0658(4) 0.4905(6) 0.0451(17) Uani 1 1 d .
H21A H 0.2073 0.0797 0.4317 0.068 Uiso 1 1 calc R
H21B H 0.2528 0.1009 0.5352 0.068 Uiso 1 1 calc R
H21C H 0.2115 0.0264 0.5113 0.068 Uiso 1 1 calc R
C12 C 0.5200(14) 0.3034(7) 0.6512(8) 0.102(4) Uani 1 1 d .
H12A H 0.5858 0.2769 0.6215 0.154 Uiso 1 1 calc R
H12B H 0.5431 0.3003 0.7175 0.154 Uiso 1 1 calc R
H12C H 0.5258 0.3492 0.6322 0.154 Uiso 1 1 calc R
O5 O 0.3835(7) 0.2799(3) 0.6259(4) 0.0577(15) Uani 1 1 d .
C13 C 0.3752(8) 0.2449(3) 0.4672(5) 0.0389(16) Uani 1 1 d .
C14 C 0.3338(9) 0.2912(4) 0.5349(5) 0.0472(18) Uani 1 1 d .
C15 C 0.2443(10) 0.3441(4) 0.5091(6) 0.055(2) Uani 1 1 d .
H15 H 0.2216 0.3739 0.5543 0.067 Uiso 1 1 calc R
C16 C 0.1874(10) 0.3539(4) 0.4173(7) 0.063(2) Uani 1 1 d .
H16 H 0.1239 0.3887 0.4014 0.076 Uiso 1 1 calc R
C17 C 0.2255(9) 0.3119(4) 0.3504(6) 0.0509(19) Uani 1 1 d .
H17 H 0.1889 0.3193 0.2887 0.061 Uiso 1 1 calc R
C18 C 0.3193(8) 0.2572(4) 0.3722(5) 0.0407(16) Uani 1 1 d .
C19 C 0.3516(7) 0.2161(4) 0.2954(5) 0.0414(17) Uani 1 1 d .
H19 H 0.3144 0.2297 0.2360 0.050 Uiso 1 1 calc R
Ni1 Ni 0.55076(8) 0.03190(4) 0.59447(5) 0.0302(3) Uani 1 1 d .
N1 N 0.7164(6) 0.0252(3) 0.6927(4) 0.0358(13) Uani 1 1 d .
O3 O 0.4617(5) -0.0388(2) 0.6740(3) 0.0352(10) Uani 1 1 d .
O6 O 0.4875(5) 0.1231(2) 0.6545(3) 0.0412(11) Uani 1 1 d .
C1 C 0.7582(16) 0.2354(7) 0.3499(8) 0.122(6) Uani 1 1 d .
H1A H 0.7556 0.2775 0.3815 0.183 Uiso 1 1 calc R
H1B H 0.6865 0.2349 0.2969 0.183 Uiso 1 1 calc R
H1C H 0.8500 0.2294 0.3297 0.183 Uiso 1 1 calc R
C2 C 0.7774(7) 0.1268(3) 0.5526(5) 0.0352(15) Uani 1 1 d .
C3 C 0.8191(8) 0.1774(4) 0.4949(5) 0.0408(16) Uani 1 1 d .
C4 C 0.9394(8) 0.2157(4) 0.5202(6) 0.0497(19) Uani 1 1 d .
H4 H 0.9662 0.2486 0.4805 0.060 Uiso 1 1 calc R
C5 C 1.0193(9) 0.2042(4) 0.6057(6) 0.059(2) Uani 1 1 d .
H5 H 1.1004 0.2296 0.6231 0.070 Uiso 1 1 calc R
C6 C 0.9802(8) 0.1557(4) 0.6651(6) 0.0466(18) Uani 1 1 d .
H6 H 1.0345 0.1488 0.7223 0.056 Uiso 1 1 calc R
C20 C 0.3864(10) 0.1279(4) 0.7192(6) 0.056(2) Uani 1 1 d .
H20A H 0.2921 0.1261 0.6864 0.084 Uiso 1 1 calc R
H20B H 0.3993 0.1694 0.7524 0.084 Uiso 1 1 calc R
H20C H 0.3996 0.0913 0.7624 0.084 Uiso 1 1 calc R
C7 C 0.8578(7) 0.1163(3) 0.6393(5) 0.0349(15) Uani 1 1 d .
C8 C 0.8259(7) 0.0643(4) 0.7045(5) 0.0391(16) Uani 1 1 d .
H8 H 0.8889 0.0589 0.7585 0.047 Uiso 1 1 calc R
C9 C 0.7073(7) -0.0312(4) 0.7556(5) 0.0411(17) Uani 1 1 d .
H9A H 0.7508 -0.0191 0.8174 0.049 Uiso 1 1 calc R
H9B H 0.7589 -0.0690 0.7346 0.049 Uiso 1 1 calc R
C10 C 0.5507(7) -0.0509(4) 0.7588(5) 0.0381(15) Uani 1 1 d .
H10 H 0.5142 -0.0252 0.8083 0.046 Uiso 1 1 calc R
C11 C 0.5445(9) -0.1263(4) 0.7827(5) 0.0439(17) Uani 1 1 d .
H11A H 0.6157 -0.1373 0.8344 0.053 Uiso 1 1 calc R
H11B H 0.4516 -0.1380 0.7992 0.053 Uiso 1 1 calc R
C22 C 0.9020(11) 0.0485(7) 0.3239(10) 0.104(5) Uani 1 1 d .
H22A H 0.9501 0.0852 0.2986 0.157 Uiso 1 1 calc R
H22B H 0.9668 0.0118 0.3365 0.157 Uiso 1 1 calc R
H22C H 0.8678 0.0623 0.3805 0.157 Uiso 1 1 calc R
C23 C 0.1837(16) 0.0520(8) 0.9065(17) 0.157(8) Uani 1 1 d .
H23 H 0.1795 0.0390 0.8410 0.188 Uiso 1 1 calc R
Cl1 Cl 0.0693(8) -0.0055(6) 0.9842(9) 0.286(5) Uani 1 1 d .
Cl2 Cl 0.1212(15) 0.1225(5) 0.9242(7) 0.302(5) Uani 1 1 d .
Cl3 Cl 0.3498(7) 0.0368(4) 0.9761(5) 0.219(3) Uani 1 1 d .
O8 O 0.7909(7) 0.0290(5) 0.2617(5) 0.094(3) Uani 1 1 d .
H8A H 0.7392 0.0040 0.2874 0.142 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'
Cl Cl 0.1484 0.1585 '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
N2 Ni2 O2 162.7(2) . .
N2 Ni2 O4 91.0(2) . .
O2 Ni2 O4 91.89(19) . .
N2 Ni2 O7 116.5(2) . .
O2 Ni2 O7 80.34(17) . .
O4 Ni2 O7 92.72(19) . .
N2 Ni2 O3 82.1(2) . 3_656
O2 Ni2 O3 97.58(18) . 3_656
O4 Ni2 O3 167.92(19) . 3_656
O7 Ni2 O3 81.55(18) . 3_656
N2 Ni2 O1 91.8(2) . .
O2 Ni2 O1 71.48(18) . .
O4 Ni2 O1 85.6(2) . .
O7 Ni2 O1 151.68(17) . .
O3 Ni2 O1 104.46(19) 3_656 .
C19 N2 C11 120.1(6) . 3_656
C19 N2 Ni2 127.4(5) . .
C11 N2 Ni2 112.5(4) 3_656 .
C3 O1 C1 118.9(7) . .
C3 O1 Ni2 109.3(4) . .
C1 O1 Ni2 129.1(6) . .
C2 O2 Ni2 122.9(4) . .
C2 O2 Ni1 126.4(4) . .
Ni2 O2 Ni1 101.77(19) . .
C13 O4 Ni2 127.4(4) . .
C21 O7 Ni1 119.5(4) . 3_656
C21 O7 Ni2 119.5(4) . .
Ni1 O7 Ni2 97.98(18) 3_656 .
C21 O7 Ni1 121.5(4) . .
Ni1 O7 Ni1 95.77(18) 3_656 .
Ni2 O7 Ni1 97.01(17) . .
C14 O5 C12 113.6(8) . .
O4 C13 C18 124.3(6) . .
O4 C13 C14 119.2(6) . .
C18 C13 C14 116.5(6) . .
O5 C14 C15 121.1(7) . .
O5 C14 C13 117.6(7) . .
C15 C14 C13 121.3(7) . .
C14 C15 C16 121.5(8) . .
C17 C16 C15 119.3(8) . .
C16 C17 C18 122.0(8) . .
C17 C18 C13 119.5(7) . .
C17 C18 C19 116.9(7) . .
C13 C18 C19 123.6(6) . .
N2 C19 C18 125.8(6) . .
N1 Ni1 O2 89.4(2) . .
N1 Ni1 O7 96.8(2) . 3_656
O2 Ni1 O7 90.62(18) . 3_656
N1 Ni1 O3 84.0(2) . .
O2 Ni1 O3 170.00(19) . .
O7 Ni1 O3 82.73(18) 3_656 .
N1 Ni1 O7 169.3(2) . .
O2 Ni1 O7 79.95(17) . .
O7 Ni1 O7 84.23(18) 3_656 .
O3 Ni1 O7 106.65(18) . .
N1 Ni1 O6 90.2(2) . .
O2 Ni1 O6 85.88(18) . .
O7 Ni1 O6 172.19(18) 3_656 .
O3 Ni1 O6 101.61(18) . .
O7 Ni1 O6 88.28(18) . .
C8 N1 C9 119.5(6) . .
C8 N1 Ni1 127.2(5) . .
C9 N1 Ni1 113.3(4) . .
C10 O3 Ni1 110.9(4) . .
C10 O3 Ni2 109.1(4) . 3_656
Ni1 O3 Ni2 96.14(19) . 3_656
C20 O6 Ni1 124.8(5) . .
O2 C2 C3 117.4(6) . .
O2 C2 C7 123.9(6) . .
C3 C2 C7 118.7(6) . .
C4 C3 O1 124.4(7) . .
C4 C3 C2 121.7(7) . .
O1 C3 C2 113.9(6) . .
C3 C4 C5 119.0(7) . .
C6 C5 C4 121.0(7) . .
C5 C6 C7 120.1(7) . .
C2 C7 C6 119.5(7) . .
C2 C7 C8 123.5(6) . .
C6 C7 C8 117.0(6) . .
N1 C8 C7 124.8(6) . .
N1 C9 C10 110.4(5) . .
O3 C10 C9 113.6(5) . .
O3 C10 C11 108.8(5) . .
C9 C10 C11 108.6(6) . .
N2 C11 C10 105.9(5) 3_656 .
Cl2 C23 Cl3 112.8(12) . .
Cl2 C23 Cl1 100.4(10) . .
Cl3 C23 Cl1 94.8(12) . .
Cl1 Cl1 C23 131.1(13) 3_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni2 N2 1.982(6) .
Ni2 O2 1.993(4) .
Ni2 O4 2.009(5) .
Ni2 O7 2.064(4) .
Ni2 O3 2.114(5) 3_656
Ni2 O1 2.383(5) .
N2 C19 1.286(9) .
N2 C11 1.479(9) 3_656
O1 C3 1.389(9) .
O1 C1 1.406(11) .
O2 C2 1.326(8) .
O2 Ni1 2.001(4) .
O4 C13 1.300(8) .
O7 C21 1.439(8) .
O7 Ni1 2.060(4) 3_656
O7 Ni1 2.073(4) .
C12 O5 1.382(13) .
O5 C14 1.364(9) .
C13 C18 1.434(10) .
C13 C14 1.439(10) .
C14 C15 1.378(11) .
C15 C16 1.387(12) .
C16 C17 1.365(12) .
C17 C18 1.420(10) .
C18 C19 1.446(10) .
Ni1 N1 1.990(6) .
Ni1 O7 2.060(4) 3_656
Ni1 O3 2.069(5) .
Ni1 O6 2.137(5) .
N1 C8 1.293(9) .
N1 C9 1.459(9) .
O3 C10 1.423(8) .
O3 Ni2 2.114(5) 3_656
O6 C20 1.426(9) .
C2 C3 1.401(10) .
C2 C7 1.403(9) .
C3 C4 1.385(10) .
C4 C5 1.390(12) .
C5 C6 1.377(12) .
C6 C7 1.414(10) .
C7 C8 1.463(10) .
C9 C10 1.543(10) .
C10 C11 1.549(10) .
C11 N2 1.479(9) 3_656
C22 O8 1.356(13) .
C23 Cl2 1.562(15) .
C23 Cl3 1.79(2) .
C23 Cl1 2.02(2) .
Cl1 Cl1 1.461(17) 3_557
