#------------------------------------------------------------------------------
#$Date: 2021-10-24 20:53:08 +0300 (Sun, 24 Oct 2021) $
#$Revision: 270074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/76/4307641.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_4307641
loop_
_publ_author_name
'Frank B. Johansson'
'Andrew D. Bond'
'Christine J. McKenzie'
_publ_contact_author_address
;
 University of Southern Denmark
 Department of Physics and Chemistry
 Campusvej 55
 5230 Odense
 Denmark
;
_publ_contact_author_email       adb@chem.sdu.dk
_publ_contact_author_fax         '+45 6615 8780'
_publ_contact_author_name        'Andrew D. Bond'
_publ_contact_author_phone       '+45 6650 2545'
_publ_section_title
;
Functional Tetrametallic Linker Modules for Coordination Polymers and
Metal-Organic Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2224
_journal_page_last               2236
_journal_paper_doi               10.1021/ic062131s
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C64 H60 Cl4 N12 O2 Zn2 2+, Cl6 Zn2 2-'
_chemical_formula_sum            'C64 H60 Cl10 N12 O2 Zn4'
_chemical_formula_weight         1645.29
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.345(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7529(9)
_cell_length_b                   27.090(2)
_cell_length_c                   12.0596(9)
_cell_measurement_reflns_used    2689
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.48
_cell_measurement_theta_min      2.60
_cell_volume                     3684.4(5)
_computing_cell_refinement       'SAINT v.5.0 (Bruker, 2001)'
_computing_data_collection       'SMART v.5.0 (Bruker, 2001)'
_computing_data_reduction        'SAINT v.5.0'
_computing_molecular_graphics    'SHELXTL v.6.10'
_computing_publication_material  'SHELXTL v.6.10'
_computing_structure_refinement  'SHELXTL v.6.10'
_computing_structure_solution    'SHELXTL v.6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'Thin slice 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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9892
_diffrn_reflns_theta_full        24.88
_diffrn_reflns_theta_max         24.88
_diffrn_reflns_theta_min         1.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.335
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.03 (Sheldrick, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0581
_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)+(0.0953P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                1925
_reflns_number_total             3282
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic062131ssi20061110_025004_2.cif
_cod_data_source_block           1_squeezed
_cod_depositor_comments
;

2021-10-24
Formula fixed to be consistent with given Z
                 miguel
;
_cod_original_formula_sum            'C64 H60 Cl10 N12 O2 Zn6'
_cod_original_formula_weight         1775.96
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               4307641
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.11019(6) 0.29037(2) 0.14691(6) 0.0481(3) Uani 1 1 d . . .
Cl1 Cl 0.21570(15) 0.23323(6) 0.08013(14) 0.0687(5) Uani 1 1 d . . .
O1 O 0.0000 0.31918(16) 0.0000 0.0424(12) Uani 1 2 d S . .
N1 N 0.0035(4) 0.24352(18) 0.2116(4) 0.0577(13) Uani 1 1 d . . .
N2 N 0.0417(4) 0.34058(16) 0.2561(4) 0.0504(12) Uani 1 1 d . . .
N3 N 0.2334(4) 0.34703(18) 0.1747(4) 0.0550(13) Uani 1 1 d . . .
C1 C -0.0250(6) 0.1985(2) 0.1715(6) 0.076(2) Uani 1 1 d . . .
H1A H 0.0080 0.1857 0.1139 0.092 Uiso 1 1 calc R . .
C2 C -0.1003(8) 0.1700(3) 0.2105(8) 0.100(3) Uani 1 1 d . . .
H2A H -0.1244 0.1386 0.1769 0.120 Uiso 1 1 calc R . .
C3 C -0.1419(7) 0.1872(4) 0.3003(11) 0.118(4) Uani 1 1 d . . .
H3A H -0.1907 0.1670 0.3324 0.142 Uiso 1 1 calc R . .
C4 C -0.1112(7) 0.2333(4) 0.3413(7) 0.099(3) Uani 1 1 d . . .
H4A H -0.1402 0.2463 0.4014 0.119 Uiso 1 1 calc R . .
C5 C -0.0376(6) 0.2615(3) 0.2951(6) 0.072(2) Uani 1 1 d . . .
C6 C 0.0052(6) 0.3117(3) 0.3423(5) 0.0690(19) Uani 1 1 d . . .
H6A H -0.0592 0.3292 0.3643 0.083 Uiso 1 1 calc R . .
H6B H 0.0729 0.3080 0.4124 0.083 Uiso 1 1 calc R . .
C7 C 0.1358(6) 0.3761(2) 0.3119(5) 0.072(2) Uani 1 1 d . . .
H7A H 0.1800 0.3636 0.3892 0.086 Uiso 1 1 calc R . .
H7B H 0.0996 0.4081 0.3222 0.086 Uiso 1 1 calc R . .
C8 C 0.2211(6) 0.3834(3) 0.2385(7) 0.072(2) Uani 1 1 d . . .
C9 C 0.2827(8) 0.4273(3) 0.2440(11) 0.147(5) Uani 1 1 d . . .
H9A H 0.2610 0.4543 0.2839 0.177 Uiso 1 1 calc R . .
C10 C 0.3632(11) 0.4330(4) 0.2004(18) 0.242(10) Uani 1 1 d . . .
H10A H 0.4146 0.4607 0.2182 0.290 Uiso 1 1 calc R . .
C11 C 0.3762(8) 0.3967(4) 0.1227(13) 0.171(6) Uani 1 1 d . . .
H11A H 0.4296 0.4019 0.0776 0.205 Uiso 1 1 calc R . .
C12 C 0.3089(6) 0.3513(3) 0.1103(7) 0.086(2) Uani 1 1 d . . .
H12A H 0.3180 0.3258 0.0592 0.104 Uiso 1 1 calc R . .
C13 C -0.0631(5) 0.3664(2) 0.1807(5) 0.0509(14) Uani 1 1 d . . .
H13A H -0.0957 0.3893 0.2278 0.061 Uiso 1 1 calc R . .
H13B H -0.1252 0.3419 0.1454 0.061 Uiso 1 1 calc R . .
C14 C 0.0000 0.3689(2) 0.0000 0.0335(16) Uani 1 2 d S . .
C15 C -0.0295(4) 0.39517(17) 0.0854(4) 0.0408(13) Uani 1 1 d . . .
C16 C -0.0300(4) 0.44538(18) 0.0838(4) 0.0405(13) Uani 1 1 d . . .
H16A H -0.0520 0.4626 0.1432 0.049 Uiso 1 1 calc R . .
C17 C 0.0000 0.4720(2) 0.0000 0.0341(16) 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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
O1 Zn1 N3 95.81(16) . . ?
O1 Zn1 N1 104.92(15) . . ?
N3 Zn1 N1 149.0(2) . . ?
O1 Zn1 N2 91.93(13) . . ?
N3 Zn1 N2 78.6(2) . . ?
N1 Zn1 N2 78.0(2) . . ?
O1 Zn1 Cl1 103.32(9) . . ?
N3 Zn1 Cl1 97.81(16) . . ?
N1 Zn1 Cl1 99.44(16) . . ?
N2 Zn1 Cl1 164.64(12) . . ?
C14 O1 Zn1 112.57(12) . 2 ?
C14 O1 Zn1 112.57(12) . . ?
Zn1 O1 Zn1 134.9(2) 2 . ?
C1 N1 C5 120.6(6) . . ?
C1 N1 Zn1 122.9(5) . . ?
C5 N1 Zn1 116.6(4) . . ?
C6 N2 C7 111.0(5) . . ?
C6 N2 C13 109.2(4) . . ?
C7 N2 C13 111.0(4) . . ?
C6 N2 Zn1 109.0(4) . . ?
C7 N2 Zn1 108.8(4) . . ?
C13 N2 Zn1 107.8(3) . . ?
C8 N3 C12 119.1(6) . . ?
C8 N3 Zn1 118.3(5) . . ?
C12 N3 Zn1 121.1(5) . . ?
N1 C1 C2 121.5(8) . . ?
N1 C1 H1A 119.3 . . ?
C2 C1 H1A 119.3 . . ?
C1 C2 C3 119.2(8) . . ?
C1 C2 H2A 120.4 . . ?
C3 C2 H2A 120.4 . . ?
C4 C3 C2 118.6(8) . . ?
C4 C3 H3A 120.7 . . ?
C2 C3 H3A 120.7 . . ?
C3 C4 C5 119.6(8) . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 H4A 120.2 . . ?
N1 C5 C4 120.4(8) . . ?
N1 C5 C6 117.7(6) . . ?
C4 C5 C6 121.8(7) . . ?
N2 C6 C5 110.5(5) . . ?
N2 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
N2 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
N2 C7 C8 110.5(5) . . ?
N2 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N3 C8 C9 122.9(8) . . ?
N3 C8 C7 116.8(6) . . ?
C9 C8 C7 120.3(8) . . ?
C10 C9 C8 123.3(12) . . ?
C10 C9 H9A 118.3 . . ?
C8 C9 H9A 118.3 . . ?
C9 C10 C11 116.6(12) . . ?
C9 C10 H10A 121.7 . . ?
C11 C10 H10A 121.7 . . ?
C10 C11 C12 120.6(10) . . ?
C10 C11 H11A 119.7 . . ?
C12 C11 H11A 119.7 . . ?
N3 C12 C11 116.4(9) . . ?
N3 C12 H12A 121.8 . . ?
C11 C12 H12A 121.8 . . ?
N2 C13 C15 110.8(4) . . ?
N2 C13 H13A 109.5 . . ?
C15 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
C15 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
O1 C14 C15 121.2(3) . 2 ?
O1 C14 C15 121.2(3) . . ?
C15 C14 C15 117.5(6) 2 . ?
C16 C15 C14 120.6(5) . . ?
C16 C15 C13 121.3(5) . . ?
C14 C15 C13 118.1(5) . . ?
C15 C16 C17 122.5(5) . . ?
C15 C16 H16A 118.7 . . ?
C17 C16 H16A 118.7 . . ?
C16 C17 C16 116.3(6) . 2 ?
C16 C17 C17 121.9(3) . 5_565 ?
C16 C17 C17 121.9(3) 2 5_565 ?
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
Zn1 O1 2.0331(18) . ?
Zn1 N3 2.071(5) . ?
Zn1 N1 2.084(5) . ?
Zn1 N2 2.197(4) . ?
Zn1 Cl1 2.2681(16) . ?
O1 C14 1.346(8) . ?
O1 Zn1 2.0331(18) 2 ?
N1 C1 1.321(8) . ?
N1 C5 1.326(8) . ?
N2 C6 1.459(7) . ?
N2 C7 1.477(8) . ?
N2 C13 1.483(6) . ?
N3 C8 1.283(8) . ?
N3 C12 1.339(8) . ?
C1 C2 1.355(10) . ?
C1 H1A 0.950 . ?
C2 C3 1.388(12) . ?
C2 H2A 0.950 . ?
C3 C4 1.356(13) . ?
C3 H3A 0.950 . ?
C4 C5 1.383(9) . ?
C4 H4A 0.950 . ?
C5 C6 1.505(10) . ?
C6 H6A 0.990 . ?
C6 H6B 0.990 . ?
C7 C8 1.525(10) . ?
C7 H7A 0.990 . ?
C7 H7B 0.990 . ?
C8 C9 1.384(10) . ?
C9 C10 1.214(15) . ?
C9 H9A 0.950 . ?
C10 C11 1.39(2) . ?
C10 H10A 0.950 . ?
C11 C12 1.449(12) . ?
C11 H11A 0.950 . ?
C12 H12A 0.950 . ?
C13 C15 1.530(7) . ?
C13 H13A 0.990 . ?
C13 H13B 0.990 . ?
C14 C15 1.374(6) 2 ?
C14 C15 1.375(6) . ?
C15 C16 1.360(6) . ?
C16 C17 1.366(6) . ?
C16 H16A 0.950 . ?
C17 C16 1.366(6) 2 ?
C17 C17 1.517(13) 5_565 ?
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
N3 Zn1 O1 C14 -31.91(16) . . . . ?
N1 Zn1 O1 C14 124.88(16) . . . . ?
N2 Zn1 O1 C14 46.78(13) . . . . ?
Cl1 Zn1 O1 C14 -131.38(5) . . . . ?
N3 Zn1 O1 Zn1 148.08(16) . . . 2 ?
N1 Zn1 O1 Zn1 -55.12(16) . . . 2 ?
N2 Zn1 O1 Zn1 -133.22(13) . . . 2 ?
Cl1 Zn1 O1 Zn1 48.61(5) . . . 2 ?
O1 Zn1 N1 C1 80.2(5) . . . . ?
N3 Zn1 N1 C1 -149.4(5) . . . . ?
N2 Zn1 N1 C1 169.0(5) . . . . ?
Cl1 Zn1 N1 C1 -26.4(5) . . . . ?
O1 Zn1 N1 C5 -98.4(4) . . . . ?
N3 Zn1 N1 C5 32.0(7) . . . . ?
N2 Zn1 N1 C5 -9.6(4) . . . . ?
Cl1 Zn1 N1 C5 155.0(4) . . . . ?
O1 Zn1 N2 C6 127.3(4) . . . . ?
N3 Zn1 N2 C6 -137.2(4) . . . . ?
N1 Zn1 N2 C6 22.5(4) . . . . ?
Cl1 Zn1 N2 C6 -59.5(7) . . . . ?
O1 Zn1 N2 C7 -111.6(3) . . . . ?
N3 Zn1 N2 C7 -16.0(3) . . . . ?
N1 Zn1 N2 C7 143.6(4) . . . . ?
Cl1 Zn1 N2 C7 61.7(7) . . . . ?
O1 Zn1 N2 C13 8.9(3) . . . . ?
N3 Zn1 N2 C13 104.4(4) . . . . ?
N1 Zn1 N2 C13 -96.0(4) . . . . ?
Cl1 Zn1 N2 C13 -177.9(4) . . . . ?
O1 Zn1 N3 C8 91.8(5) . . . . ?
N1 Zn1 N3 C8 -40.4(7) . . . . ?
N2 Zn1 N3 C8 1.1(5) . . . . ?
Cl1 Zn1 N3 C8 -163.8(5) . . . . ?
O1 Zn1 N3 C12 -74.5(5) . . . . ?
N1 Zn1 N3 C12 153.2(4) . . . . ?
N2 Zn1 N3 C12 -165.3(5) . . . . ?
Cl1 Zn1 N3 C12 29.8(5) . . . . ?
C5 N1 C1 C2 2.6(10) . . . . ?
Zn1 N1 C1 C2 -175.9(5) . . . . ?
N1 C1 C2 C3 -4.6(12) . . . . ?
C1 C2 C3 C4 4.0(13) . . . . ?
C2 C3 C4 C5 -1.6(13) . . . . ?
C1 N1 C5 C4 -0.1(9) . . . . ?
Zn1 N1 C5 C4 178.6(5) . . . . ?
C1 N1 C5 C6 175.9(5) . . . . ?
Zn1 N1 C5 C6 -5.5(7) . . . . ?
C3 C4 C5 N1 -0.4(11) . . . . ?
C3 C4 C5 C6 -176.2(7) . . . . ?
C7 N2 C6 C5 -150.7(5) . . . . ?
C13 N2 C6 C5 86.6(6) . . . . ?
Zn1 N2 C6 C5 -30.9(6) . . . . ?
N1 C5 C6 N2 25.4(8) . . . . ?
C4 C5 C6 N2 -158.7(6) . . . . ?
C6 N2 C7 C8 146.7(5) . . . . ?
C13 N2 C7 C8 -91.6(6) . . . . ?
Zn1 N2 C7 C8 26.8(5) . . . . ?
C12 N3 C8 C9 0.1(11) . . . . ?
Zn1 N3 C8 C9 -166.6(7) . . . . ?
C12 N3 C8 C7 -178.7(5) . . . . ?
Zn1 N3 C8 C7 14.6(7) . . . . ?
N2 C7 C8 N3 -28.4(8) . . . . ?
N2 C7 C8 C9 152.7(7) . . . . ?
N3 C8 C9 C10 -9(2) . . . . ?
C7 C8 C9 C10 169.6(14) . . . . ?
C8 C9 C10 C11 13(2) . . . . ?
C9 C10 C11 C12 -10(2) . . . . ?
C8 N3 C12 C11 2.9(10) . . . . ?
Zn1 N3 C12 C11 169.2(6) . . . . ?
C10 C11 C12 N3 1.5(15) . . . . ?
C6 N2 C13 C15 -177.3(5) . . . . ?
C7 N2 C13 C15 60.0(6) . . . . ?
Zn1 N2 C13 C15 -59.0(5) . . . . ?
Zn1 O1 C14 C15 -57.9(2) 2 . . 2 ?
Zn1 O1 C14 C15 122.1(2) . . . 2 ?
Zn1 O1 C14 C15 122.1(2) 2 . . . ?
Zn1 O1 C14 C15 -57.9(2) . . . . ?
O1 C14 C15 C16 -179.5(3) . . . . ?
C15 C14 C15 C16 0.5(3) 2 . . . ?
O1 C14 C15 C13 -0.3(5) . . . . ?
C15 C14 C15 C13 179.7(5) 2 . . . ?
N2 C13 C15 C16 -111.6(5) . . . . ?
N2 C13 C15 C14 69.2(6) . . . . ?
C14 C15 C16 C17 -1.1(7) . . . . ?
C13 C15 C16 C17 179.8(4) . . . . ?
C15 C16 C17 C16 0.5(3) . . . 2 ?
C15 C16 C17 C17 -179.5(3) . . . 5_565 ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.013 0.000 0.004 503 166
2 -0.015 0.500 0.496 503 166
