#------------------------------------------------------------------------------
#$Date: 2021-04-16 11:46:56 +0300 (Fri, 16 Apr 2021) $
#$Revision: 264242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/50/35/4503575.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_4503575
loop_
_publ_author_name
'Xu, Qiang'
'Zou, Ru-Qiang'
'Zhong, Rui-Qin'
'Kachi-Terajima, Chihiro'
'Takamizawa, Satoshi'
_publ_section_title
;
 Cubic Metal−Organic Polyhedrons of Nickel(II)
 Imidazoledicarboxylate Depositing Protons or Alkali Metal Ions
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2458
_journal_paper_doi               10.1021/cg8000762
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C76 H116 N24 Ni8 O74'
_chemical_formula_weight         3019.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           69
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8543(14)
_cell_length_b                   25.4617(14)
_cell_length_c                   28.331(2)
_cell_measurement_reflns_used    1652
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      2.45
_cell_volume                     14322.0(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL(Sheldrick, 1997b)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      183(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       'φ and δ 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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            18471
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.9778
_exptl_absorpt_correction_T_min  0.7657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6224
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.808
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.00009(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3383
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1656P)²+76.1475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2511
_reflns_number_gt                2444
_reflns_number_total             3383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg8000762-file003.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2021-04-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C38 H58 N12 Ni4 O37'
_cod_original_formula_weight         1509.80
_cod_original_formula_units_Z            8
_cod_original_cell_volume        14322.2(18)
_cod_original_sg_symbol_H-M      Fmmm
_cod_database_code               4503575
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, 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
Ni1 Ni 0.15921(3) 0.37680(3) 0.11205(2) 0.0450(4) Uani 1 1 d .
C1 C 0.1292(4) 0.5000 0.1155(2) 0.0438(17) Uani 1 2 d S
H1 H 0.0817 0.5000 0.1113 0.053 Uiso 1 2 calc SR
C2 C 0.2302(3) 0.4727(2) 0.12510(18) 0.0477(13) Uani 1 1 d .
C3 C 0.2829(3) 0.4316(3) 0.1289(2) 0.0605(16) Uani 1 1 d .
C4 C 0.1627(4) 0.4028(3) 0.0000 0.0457(18) Uani 1 2 d S
H4 H 0.1587 0.4400 0.0000 0.055 Uiso 1 2 calc SR
C5 C 0.1703(3) 0.3238(2) 0.0242(2) 0.0478(13) Uani 1 1 d .
C6 C 0.1737(3) 0.2814(2) 0.0592(2) 0.0540(15) Uani 1 1 d .
C7 C 0.0000 0.3746(3) 0.0894(3) 0.0467(18) Uani 1 2 d S
H7 H 0.0000 0.3800 0.0563 0.056 Uiso 1 2 calc SR
C8 C 0.0351(3) 0.3633(3) 0.1594(2) 0.0589(15) Uani 1 1 d .
C9 C 0.0795(4) 0.3598(4) 0.2003(3) 0.084(2) Uani 1 1 d D
C10 C 0.3151(6) 0.2972(4) 0.1981(3) 0.103(3) Uani 1 1 d .
H10A H 0.3343 0.2649 0.2111 0.154 Uiso 1 1 calc R
H10B H 0.2659 0.2950 0.1986 0.154 Uiso 1 1 calc R
H10C H 0.3298 0.3273 0.2171 0.154 Uiso 1 1 calc R
C11 C 0.3389(3) 0.3042(3) 0.1481(3) 0.0637(18) Uani 1 1 d .
H11A H 0.3265 0.2728 0.1294 0.076 Uiso 1 1 calc R
H11B H 0.3161 0.3350 0.1340 0.076 Uiso 1 1 calc R
N1 N 0.1656(2) 0.45634(19) 0.11873(16) 0.0453(11) Uani 1 1 d .
N2 N 0.1658(2) 0.37420(16) 0.03972(17) 0.0439(11) Uani 1 1 d .
N3 N 0.0563(3) 0.37040(18) 0.11476(16) 0.0467(12) Uani 1 1 d .
O1 O 0.2617(2) 0.38471(17) 0.12240(17) 0.0604(11) Uani 1 1 d .
O2 O 0.3421(2) 0.4422(3) 0.1386(3) 0.097(2) Uani 1 1 d .
H2A H 0.3470 0.4750 0.1393 0.146 Uiso 1 1 calc R
O3 O 0.1732(2) 0.29332(17) 0.10180(17) 0.0608(11) Uani 1 1 d .
O4 O 0.1746(2) 0.23394(15) 0.04415(18) 0.0639(12) Uani 1 1 d .
H4A H 0.164(5) 0.238(4) 0.0000 0.07(3) Uiso 1 2 d S
O5 O 0.1455(2) 0.3619(2) 0.18687(18) 0.0731(13) Uani 1 1 d .
O6 O 0.0667(3) 0.3523(4) 0.23868(19) 0.127(3) Uani 1 1 d .
H6A H 0.0246 0.3516 0.2420 0.190 Uiso 1 1 calc RD
O7 O 0.4124(5) 0.3118(6) 0.1461(4) 0.177(4) Uani 1 1 d .
H7A H 0.4231 0.3241 0.1196 0.266 Uiso 1 1 calc R
O1W O 0.1473(13) 0.1042(8) 0.0000 0.305(13) Uani 1 2 d S
O2W O 0.2500 0.4265(10) 0.2500 0.264(10) Uani 1 2 d S
O3W O 0.433(2) 0.5000 0.137(2) 0.45(3) Uani 1 2 d S
O4W O 0.0000 0.2463(19) 0.0000 0.48(4) Uani 1 4 d S
O5W O 0.5000 0.551(2) 0.151(3) 0.69(5) Uani 1 2 d S
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
N1 Ni1 N3 97.88(18) . .
N1 Ni1 N2 96.93(17) . .
N3 Ni1 N2 95.64(18) . .
N1 Ni1 O1 80.14(18) . .
N3 Ni1 O1 169.6(2) . .
N2 Ni1 O1 94.71(19) . .
N1 Ni1 O3 168.81(19) . .
N3 Ni1 O3 93.15(18) . .
N2 Ni1 O3 80.00(17) . .
O1 Ni1 O3 89.34(18) . .
N1 Ni1 O5 95.2(2) . .
N3 Ni1 O5 79.88(18) . .
N2 Ni1 O5 167.6(2) . .
O1 Ni1 O5 90.12(19) . .
O3 Ni1 O5 88.6(2) . .
N1 C1 N1 113.6(7) . 19_565
N1 C1 H1 123.2 . .
N1 C1 H1 123.2 19_565 .
N1 C2 C2 107.9(3) . 19_565
N1 C2 C3 117.3(5) . .
C2 C2 C3 134.9(3) 19_565 .
O2 C3 O1 123.3(6) . .
O2 C3 C2 122.1(6) . .
O1 C3 C2 114.6(5) . .
N2 C4 N2 114.0(6) 18 .
N2 C4 H4 123.0 18 .
N2 C4 H4 123.0 . .
N2 C5 C5 108.9(3) . 18
N2 C5 C6 118.6(5) . .
C5 C5 C6 132.5(3) 18 .
O3 C6 O4 123.6(6) . .
O3 C6 C5 118.3(5) . .
O4 C6 C5 118.1(6) . .
N3 C7 N3 114.0(7) 20 .
N3 C7 H7 123.0 20 .
N3 C7 H7 123.0 . .
N3 C8 C8 108.2(3) . 20
N3 C8 C9 124.5(6) . .
C8 C8 C9 127.2(4) 20 .
O6 C9 O5 119.3(7) . .
O6 C9 C8 129.5(7) . .
O5 C9 C8 110.8(6) . .
C11 C10 H10A 109.5 . .
C11 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C11 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O7 C11 C10 111.3(8) . .
O7 C11 H11A 109.4 . .
C10 C11 H11A 109.4 . .
O7 C11 H11B 109.4 . .
C10 C11 H11B 109.4 . .
H11A C11 H11B 108.0 . .
C1 N1 C2 105.4(5) . .
C1 N1 Ni1 142.3(4) . .
C2 N1 Ni1 112.0(4) . .
C4 N2 C5 104.1(5) . .
C4 N2 Ni1 144.7(4) . .
C5 N2 Ni1 111.0(4) . .
C7 N3 C8 104.8(5) . .
C7 N3 Ni1 144.0(4) . .
C8 N3 Ni1 110.9(4) . .
C3 O1 Ni1 115.8(4) . .
C3 O2 H2A 109.5 . .
C6 O3 Ni1 111.8(4) . .
C6 O4 H4A 104(5) . .
C9 O5 Ni1 113.6(4) . .
C9 O6 H6A 109.5 . .
C11 O7 H7A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.038(5) .
Ni1 N3 2.052(5) .
Ni1 N2 2.054(5) .
Ni1 O1 2.065(5) .
Ni1 O3 2.163(4) .
Ni1 O5 2.171(5) .
C1 N1 1.329(6) .
C1 N1 1.329(6) 19_565
C1 H1 0.9500 .
C2 N1 1.361(7) .
C2 C2 1.389(11) 19_565
C2 C3 1.485(8) .
C3 O2 1.237(8) .
C3 O1 1.279(8) .
C4 N2 1.342(6) 18
C4 N2 1.342(6) .
C4 H4 0.9500 .
C5 N2 1.359(7) .
C5 C5 1.370(12) 18
C5 C6 1.468(8) .
C6 O3 1.246(8) .
C6 O4 1.280(7) .
C7 N3 1.332(6) 20
C7 N3 1.332(6) .
C7 H7 0.9500 .
C8 N3 1.346(8) .
C8 C8 1.392(12) 20
C8 C9 1.459(10) .
C9 O6 1.132(7) .
C9 O5 1.365(9) .
C10 C11 1.502(12) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 O7 1.475(11) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
O2 H2A 0.8400 .
O4 H4A 1.273(18) .
O6 H6A 0.8400 .
O7 H7A 0.8400 .
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
N1 C2 C3 O2 -173.9(7) .
C2 C2 C3 O2 8.4(10) 19_565
N1 C2 C3 O1 4.6(8) .
C2 C2 C3 O1 -173.1(3) 19_565
N2 C5 C6 O3 -1.0(8) .
C5 C5 C6 O3 179.5(4) 18
N2 C5 C6 O4 176.7(5) .
C5 C5 C6 O4 -2.8(8) 18
N3 C8 C9 O6 -177.2(10) .
C8 C8 C9 O6 7.2(14) 20
N3 C8 C9 O5 -3.3(11) .
C8 C8 C9 O5 -178.9(4) 20
N1 C1 N1 C2 0.8(8) 19_565
N1 C1 N1 Ni1 -172.1(2) 19_565
C2 C2 N1 C1 -0.5(5) 19_565
C3 C2 N1 C1 -178.8(5) .
C2 C2 N1 Ni1 174.84(16) 19_565
C3 C2 N1 Ni1 -3.5(6) .
N3 Ni1 N1 C1 -16.4(7) .
N2 Ni1 N1 C1 80.3(7) .
O1 Ni1 N1 C1 173.9(7) .
O3 Ni1 N1 C1 153.6(9) .
O5 Ni1 N1 C1 -96.9(7) .
N3 Ni1 N1 C2 171.0(4) .
N2 Ni1 N1 C2 -92.3(4) .
O1 Ni1 N1 C2 1.3(4) .
O3 Ni1 N1 C2 -19.0(11) .
O5 Ni1 N1 C2 90.5(4) .
N2 C4 N2 C5 -0.8(8) 18
N2 C4 N2 Ni1 -174.0(2) 18
C5 C5 N2 C4 0.4(5) 18
C6 C5 N2 C4 -179.1(5) .
C5 C5 N2 Ni1 176.24(15) 18
C6 C5 N2 Ni1 -3.3(6) .
N1 Ni1 N2 C4 -13.8(8) .
N3 Ni1 N2 C4 84.9(8) .
O1 Ni1 N2 C4 -94.4(8) .
O3 Ni1 N2 C4 177.1(8) .
O5 Ni1 N2 C4 153.1(9) .
N1 Ni1 N2 C5 173.3(4) .
N3 Ni1 N2 C5 -88.0(4) .
O1 Ni1 N2 C5 92.7(4) .
O3 Ni1 N2 C5 4.2(4) .
O5 Ni1 N2 C5 -19.9(10) .
N3 C7 N3 C8 -0.2(8) 20
N3 C7 N3 Ni1 -172.9(2) 20
C8 C8 N3 C7 0.1(5) 20
C9 C8 N3 C7 -176.1(7) .
C8 C8 N3 Ni1 175.50(15) 20
C9 C8 N3 Ni1 -0.8(9) .
N1 Ni1 N3 C7 81.3(7) .
N2 Ni1 N3 C7 -16.5(7) .
O1 Ni1 N3 C7 159.6(9) .
O3 Ni1 N3 C7 -96.8(7) .
O5 Ni1 N3 C7 175.2(7) .
N1 Ni1 N3 C8 -91.1(4) .
N2 Ni1 N3 C8 171.1(4) .
O1 Ni1 N3 C8 -12.8(12) .
O3 Ni1 N3 C8 90.9(4) .
O5 Ni1 N3 C8 2.8(4) .
O2 C3 O1 Ni1 175.2(6) .
C2 C3 O1 Ni1 -3.4(7) .
N1 Ni1 O1 C3 1.3(5) .
N3 Ni1 O1 C3 -78.6(11) .
N2 Ni1 O1 C3 97.5(5) .
O3 Ni1 O1 C3 177.4(5) .
O5 Ni1 O1 C3 -94.0(5) .
O4 C6 O3 Ni1 -173.0(5) .
C5 C6 O3 Ni1 4.6(7) .
N1 Ni1 O3 C6 -79.9(11) .
N3 Ni1 O3 C6 90.2(4) .
N2 Ni1 O3 C6 -4.9(4) .
O1 Ni1 O3 C6 -99.8(4) .
O5 Ni1 O3 C6 170.0(4) .
O6 C9 O5 Ni1 -180.0(9) .
C8 C9 O5 Ni1 5.4(9) .
N1 Ni1 O5 C9 92.3(6) .
N3 Ni1 O5 C9 -4.8(6) .
N2 Ni1 O5 C9 -74.6(10) .
O1 Ni1 O5 C9 172.4(6) .
O3 Ni1 O5 C9 -98.3(6) .
