#------------------------------------------------------------------------------
#$Date: 2023-12-12 11:56:26 +0200 (Tue, 12 Dec 2023) $
#$Revision: 288243 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/61/4326122.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_4326122
loop_
_publ_author_name
'Robert M. Haak'
'Antonello Decortes'
'Eduardo C. Escudero-Adán'
'Marta Martínez Belmonte'
'Eddy Martin'
'Jordi Benet-Buchholz'
'Arjan W. Kleij'
_publ_section_title
;
 Shape-Persistent Octanuclear Zinc Salen Clusters: Synthesis,
 Characterization, and Catalysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7934
_journal_page_last               7936
_journal_paper_doi               10.1021/ic201064d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C92 H80 N12 O24 Zn8'
_chemical_formula_weight         2260.64
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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            2
_cell_length_a                   18.2189(18)
_cell_length_b                   18.2189(18)
_cell_length_c                   13.4500(15)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.24
_cell_volume                     4464.4(8)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR2008
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            79713
_diffrn_reflns_theta_full        26.27
_diffrn_reflns_theta_max         26.27
_diffrn_reflns_theta_min         1.88
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_T_max  0.8921
_exptl_absorpt_correction_T_min  0.8702
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0388
_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)+(0.0462P)²+11.9492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                3667
_reflns_number_total             4517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201064d_si_004.cif
_cod_data_source_block           mo_rmh492_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suppport' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4326122
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -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
Zn1 Zn 0.15941(2) 0.14949(2) 0.25496(3) 0.02322(13) Uani 1 1 d .
Zn2 Zn 0.04135(2) 0.23129(2) 0.06936(3) 0.02422(13) Uani 1 1 d .
N1 N -0.03489(17) 0.16558(18) -0.0071(2) 0.0266(7) Uani 1 1 d .
N2 N 0.04449(17) 0.27435(19) -0.0722(2) 0.0282(7) Uani 1 1 d .
O1 O 0.10949(14) 0.05825(15) 0.2976(2) 0.0293(6) Uani 1 1 d .
O2 O 0.06776(13) 0.14690(14) 0.15600(19) 0.0259(5) Uani 1 1 d .
O3 O 0.14318(14) 0.24760(13) 0.31888(19) 0.0262(6) Uani 1 1 d .
O4 O 0.21455(14) 0.13535(14) 0.39767(18) 0.0258(5) Uani 1 1 d .
O5 O -0.03175(14) 0.29321(14) 0.14278(19) 0.0269(6) Uani 1 1 d .
H5 H -0.0440 0.2722 0.1941 0.040 Uiso 1 1 calc R
C1 C 0.0557(2) 0.0349(2) 0.2388(3) 0.0260(8) Uani 1 1 d .
C2 C 0.0228(2) -0.0337(2) 0.2504(3) 0.0301(8) Uani 1 1 d .
H2 H 0.0391 -0.0650 0.3004 0.036 Uiso 1 1 calc R
C3 C -0.0333(2) -0.0559(2) 0.1888(3) 0.0336(9) Uani 1 1 d .
H3 H -0.0553 -0.1015 0.1979 0.040 Uiso 1 1 calc R
C4 C -0.0567(2) -0.0106(2) 0.1143(3) 0.0317(9) Uani 1 1 d .
H4 H -0.0938 -0.0265 0.0720 0.038 Uiso 1 1 calc R
C5 C -0.0259(2) 0.0597(2) 0.1000(3) 0.0269(8) Uani 1 1 d .
C6 C 0.03163(19) 0.0830(2) 0.1624(3) 0.0250(8) Uani 1 1 d .
C7 C -0.0532(2) 0.0996(2) 0.0154(3) 0.0280(8) Uani 1 1 d .
H7 H -0.0865 0.0759 -0.0260 0.034 Uiso 1 1 calc R
C8 C -0.0624(2) 0.2009(2) -0.0929(3) 0.0291(8) Uani 1 1 d .
C9 C -0.1268(2) 0.1825(2) -0.1427(3) 0.0323(9) Uani 1 1 d .
H9 H -0.1551 0.1432 -0.1209 0.039 Uiso 1 1 calc R
C10 C -0.1487(2) 0.2226(2) -0.2245(3) 0.0381(10) Uani 1 1 d .
H10 H -0.1912 0.2097 -0.2584 0.046 Uiso 1 1 calc R
C11 C -0.1075(2) 0.2823(3) -0.2566(3) 0.0388(10) Uani 1 1 d .
H11 H -0.1230 0.3095 -0.3111 0.047 Uiso 1 1 calc R
C12 C -0.0436(2) 0.3012(2) -0.2075(3) 0.0330(9) Uani 1 1 d .
H12 H -0.0166 0.3417 -0.2284 0.040 Uiso 1 1 calc R
C13 C -0.0198(2) 0.2598(2) -0.1273(3) 0.0280(8) Uani 1 1 d .
C14 C 0.1012(2) 0.3027(3) -0.1132(3) 0.0355(10) Uani 1 1 d .
H14 H 0.0991 0.3096 -0.1817 0.043 Uiso 1 1 calc R
C15 C 0.1674(2) 0.3250(3) -0.0645(3) 0.0375(10) Uani 1 1 d .
C16 C 0.1805(2) 0.1794(2) 0.4600(3) 0.0293(8) Uani 1 1 d .
C17 C 0.1439(2) 0.2412(2) 0.4194(3) 0.0318(9) Uani 1 1 d .
C18 C 0.1095(3) 0.2911(3) 0.4807(3) 0.0461(12) Uani 1 1 d .
H18 H 0.0859 0.3316 0.4534 0.055 Uiso 1 1 calc R
C19 C 0.1099(4) 0.2812(3) 0.5838(4) 0.0646(18) Uani 1 1 d .
H19 H 0.0884 0.3163 0.6248 0.077 Uiso 1 1 calc R
C20 C 0.1415(3) 0.2204(3) 0.6247(3) 0.0532(14) Uani 1 1 d .
H20 H 0.1408 0.2141 0.6933 0.064 Uiso 1 1 calc R
N1S N 0.9349(2) 0.1562(2) 0.4374(3) 0.0374(8) Uani 1 1 d .
O1S O 0.91463(17) 0.23380(17) 0.3085(2) 0.0429(8) Uani 1 1 d .
C1S C 0.9520(2) 0.1880(2) 0.3513(3) 0.0362(10) Uani 1 1 d .
H1S H 0.9959 0.1742 0.3214 0.043 Uiso 1 1 calc R
C2S C 0.8681(3) 0.1761(3) 0.4885(4) 0.0449(11) Uani 1 1 d .
H2S1 H 0.8792 0.2098 0.5412 0.067 Uiso 1 1 calc R
H2S2 H 0.8458 0.1328 0.5158 0.067 Uiso 1 1 calc R
H2S3 H 0.8348 0.1988 0.4425 0.067 Uiso 1 1 calc R
C3S C 0.9845(3) 0.1047(4) 0.4837(4) 0.0696(18) Uani 1 1 d .
H3S1 H 1.0252 0.0955 0.4401 0.104 Uiso 1 1 calc R
H3S2 H 0.9591 0.0596 0.4968 0.104 Uiso 1 1 calc R
H3S3 H 1.0023 0.1249 0.5451 0.104 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'
Zn Zn 0.2839 1.4301 '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
O3 Zn1 O1 119.51(11) 8_656 .
O3 Zn1 O3 113.30(15) 8_656 .
O1 Zn1 O3 123.83(11) . .
O3 Zn1 O2 110.94(10) 8_656 .
O1 Zn1 O2 78.62(10) . .
O3 Zn1 O2 99.88(10) . .
O3 Zn1 O4 92.33(10) 8_656 .
O1 Zn1 O4 81.82(10) . .
O3 Zn1 O4 78.23(10) . .
O2 Zn1 O4 154.91(10) . .
O2 Zn2 O5 107.89(10) . .
O2 Zn2 O4 92.51(10) . 7_566
O5 Zn2 O4 100.35(11) . 7_566
O2 Zn2 N2 146.04(12) . .
O5 Zn2 N2 105.03(12) . .
O4 Zn2 N2 89.62(11) 7_566 .
O2 Zn2 N1 90.34(11) . .
O5 Zn2 N1 97.03(11) . .
O4 Zn2 N1 160.58(11) 7_566 .
N2 Zn2 N1 77.49(13) . .
C7 N1 C8 121.7(3) . .
C7 N1 Zn2 126.2(3) . .
C8 N1 Zn2 112.0(2) . .
C14 N2 C13 121.2(3) . .
C14 N2 Zn2 125.1(3) . .
C13 N2 Zn2 113.0(2) . .
C1 O1 Zn1 115.8(2) . .
C6 O2 Zn2 126.2(2) . .
C6 O2 Zn1 111.3(2) . .
Zn2 O2 Zn1 122.50(12) . .
C17 O3 Zn1 125.2(2) . 7_566
C17 O3 Zn1 110.4(2) . .
Zn1 O3 Zn1 122.86(13) 7_566 .
C16 O4 Zn2 127.3(2) . 8_656
C16 O4 Zn1 105.8(2) . .
Zn2 O4 Zn1 121.12(12) 8_656 .
O1 C1 C2 122.5(3) . .
O1 C1 C6 117.4(3) . .
C2 C1 C6 120.1(4) . .
C3 C2 C1 121.0(4) . .
C4 C3 C2 119.7(4) . .
C3 C4 C5 121.6(4) . .
C6 C5 C4 119.2(4) . .
C6 C5 C7 125.2(3) . .
C4 C5 C7 115.4(3) . .
O2 C6 C5 126.1(3) . .
O2 C6 C1 115.5(3) . .
C5 C6 C1 118.4(3) . .
N1 C7 C5 124.7(4) . .
C9 C8 C13 119.4(4) . .
C9 C8 N1 125.7(4) . .
C13 C8 N1 114.9(3) . .
C10 C9 C8 120.0(4) . .
C9 C10 C11 120.5(4) . .
C12 C11 C10 120.1(4) . .
C11 C12 C13 120.0(4) . .
C12 C13 C8 119.9(4) . .
C12 C13 N2 124.6(4) . .
C8 C13 N2 115.4(3) . .
N2 C14 C15 126.7(4) . .
C20 C15 C16 119.7(4) 7_566 7_566
C20 C15 C14 116.1(4) 7_566 .
C16 C15 C14 124.0(4) 7_566 .
O4 C16 C17 117.4(3) . .
O4 C16 C15 124.6(4) . 8_656
C17 C16 C15 117.9(3) . 8_656
O3 C17 C18 122.3(4) . .
O3 C17 C16 117.2(3) . .
C18 C17 C16 120.5(4) . .
C17 C18 C19 120.4(4) . .
C20 C19 C18 120.4(4) . .
C19 C20 C15 120.7(4) . 8_656
C1S N1S C3S 120.8(4) . .
C1S N1S C2S 120.2(4) . .
C3S N1S C2S 119.0(4) . .
O1S C1S N1S 125.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O3 1.967(2) 8_656
Zn1 O1 1.980(3) .
Zn1 O3 2.005(3) .
Zn1 O2 2.136(3) .
Zn1 O4 2.182(3) .
Zn2 O2 1.988(3) .
Zn2 O5 2.005(3) .
Zn2 O4 2.026(3) 7_566
Zn2 N2 2.060(3) .
Zn2 N1 2.102(3) .
N1 C7 1.283(5) .
N1 C8 1.413(5) .
N2 C14 1.280(5) .
N2 C13 1.411(5) .
O1 C1 1.328(5) .
O2 C6 1.340(4) .
O3 C17 1.357(5) .
O3 Zn1 1.967(2) 7_566
O4 C16 1.315(4) .
O4 Zn2 2.026(3) 8_656
C1 C2 1.395(5) .
C1 C6 1.421(5) .
C2 C3 1.377(6) .
C3 C4 1.365(6) .
C4 C5 1.412(5) .
C5 C6 1.407(5) .
C5 C7 1.439(5) .
C8 C9 1.392(5) .
C8 C13 1.405(6) .
C9 C10 1.379(6) .
C10 C11 1.388(6) .
C11 C12 1.383(6) .
C12 C13 1.386(6) .
C14 C15 1.432(6) .
C15 C20 1.400(6) 7_566
C15 C16 1.426(5) 7_566
C16 C17 1.418(5) .
C16 C15 1.426(5) 8_656
C17 C18 1.379(6) .
C18 C19 1.398(6) .
C19 C20 1.365(7) .
C20 C15 1.400(6) 8_656
N1S C1S 1.331(5) .
N1S C3S 1.445(6) .
N1S C2S 1.445(5) .
O1S C1S 1.220(5) .
