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#$Date: 2019-11-25 01:51:11 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239903 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/04/4350478.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_4350478
loop_
_publ_author_name
'Custelcean, Radu'
'Haverlock, Tamara J.'
'Moyer, Bruce A.'
_publ_section_title
;
 Anion separation by selective crystallization of metal-organic
 frameworks.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6446
_journal_page_last               6452
_journal_paper_doi               10.1021/ic060958g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C11 H10 I2 N4 O Zn'
_chemical_formula_weight         533.40
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 104.884(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1499(11)
_cell_length_b                   17.1161(19)
_cell_length_c                   8.7576(10)
_cell_measurement_temperature    173(2)
_cell_volume                     1470.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17677
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    5.866
_exptl_absorpt_correction_T_max  0.4020
_exptl_absorpt_correction_T_min  0.1823
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0174P)²+1.6306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0480
_reflns_number_gt                3610
_reflns_number_total             3661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060958gsi20060531_050744.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      p21/c
_cod_database_code               4350478
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
I1 I 0.476741(16) 0.836630(10) 0.915541(19) 0.02745(5) Uani 1 1 d .
Zn1 Zn 0.26615(3) 0.891691(16) 0.71738(3) 0.02038(6) Uani 1 1 d .
I2 I 0.135924(17) 1.008430(9) 0.78728(2) 0.02742(5) Uani 1 1 d .
N1 N 0.13559(19) 0.80060(12) 0.6313(2) 0.0213(4) Uani 1 1 d .
N2 N -0.66867(19) 0.91879(12) 0.5202(2) 0.0204(4) Uani 1 1 d .
C4 C -0.0783(2) 0.75948(14) 0.4631(3) 0.0201(4) Uani 1 1 d .
C11 C -0.5582(2) 0.88259(14) 0.4958(3) 0.0212(4) Uani 1 1 d .
H11 H -0.5122 0.8449 0.5701 0.025 Uiso 1 1 calc R
C7 C -0.7343(2) 0.97173(15) 0.4151(3) 0.0253(5) Uani 1 1 d .
H7 H -0.8130 0.9966 0.4322 0.030 Uiso 1 1 calc R
C5 C 0.0085(2) 0.81678(14) 0.5463(3) 0.0212(4) Uani 1 1 d .
H5 H -0.0234 0.8691 0.5429 0.025 Uiso 1 1 calc R
C1 C 0.1802(3) 0.72637(15) 0.6363(3) 0.0276(5) Uani 1 1 d .
H1 H 0.2694 0.7144 0.6979 0.033 Uiso 1 1 calc R
O1 O -0.27591(17) 0.82977(10) 0.5865(2) 0.0238(3) Uani 1 1 d .
N3 N -0.20920(19) 0.78136(12) 0.3744(2) 0.0224(4) Uani 1 1 d .
H3N H -0.2372 0.7678 0.2743 0.027 Uiso 1 1 calc R
C10 C -0.5096(2) 0.89890(13) 0.3648(3) 0.0197(4) Uani 1 1 d .
C6 C -0.2940(2) 0.82394(13) 0.4433(3) 0.0194(4) Uani 1 1 d .
C8 C -0.6913(3) 0.99115(15) 0.2834(3) 0.0275(5) Uani 1 1 d .
H8 H -0.7395 1.0290 0.2110 0.033 Uiso 1 1 calc R
C9 C -0.5767(3) 0.95492(14) 0.2573(3) 0.0240(5) Uani 1 1 d .
H9 H -0.5447 0.9681 0.1678 0.029 Uiso 1 1 calc R
C3 C -0.0312(3) 0.68353(15) 0.4653(3) 0.0286(5) Uani 1 1 d .
H3 H -0.0873 0.6435 0.4073 0.034 Uiso 1 1 calc R
C2 C 0.1002(3) 0.66724(15) 0.5546(4) 0.0337(6) Uani 1 1 d .
H2 H 0.1348 0.6155 0.5593 0.040 Uiso 1 1 calc R
N4 N -0.3975(2) 0.85976(13) 0.3346(2) 0.0228(4) Uani 1 1 d .
H4N H -0.3934 0.8580 0.2356 0.027 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'
I I -0.4742 1.8119 '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 Zn1 N1 100.32(8) 1_655 .
N2 Zn1 I2 108.84(6) 1_655 .
N1 Zn1 I2 110.84(6) . .
N2 Zn1 I1 105.05(5) 1_655 .
N1 Zn1 I1 108.42(6) . .
I2 Zn1 I1 121.215(13) . .
C5 N1 C1 118.7(2) . .
C5 N1 Zn1 118.90(16) . .
C1 N1 Zn1 121.56(16) . .
C7 N2 C11 119.3(2) . .
C7 N2 Zn1 121.28(16) . 1_455
C11 N2 Zn1 119.43(16) . 1_455
C3 C4 C5 119.0(2) . .
C3 C4 N3 122.1(2) . .
C5 C4 N3 118.8(2) . .
N2 C11 C10 121.7(2) . .
N2 C7 C8 122.0(2) . .
N1 C5 C4 122.2(2) . .
N1 C1 C2 121.9(2) . .
C6 N3 C4 120.39(19) . .
C11 C10 C9 118.8(2) . .
C11 C10 N4 122.5(2) . .
C9 C10 N4 118.8(2) . .
O1 C6 N4 124.2(2) . .
O1 C6 N3 123.0(2) . .
N4 C6 N3 112.7(2) . .
C7 C8 C9 119.4(2) . .
C8 C9 C10 118.8(2) . .
C4 C3 C2 118.3(2) . .
C1 C2 C3 119.8(2) . .
C6 N4 C10 126.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Zn1 2.5618(4) .
Zn1 N2 2.054(2) 1_655
Zn1 N1 2.060(2) .
Zn1 I2 2.5554(4) .
N1 C5 1.342(3) .
N1 C1 1.346(3) .
N2 C7 1.341(3) .
N2 C11 1.346(3) .
N2 Zn1 2.054(2) 1_455
C4 C3 1.383(3) .
C4 C5 1.392(3) .
C4 N3 1.407(3) .
C11 C10 1.389(3) .
C7 C8 1.375(4) .
C1 C2 1.377(4) .
O1 C6 1.224(3) .
N3 C6 1.379(3) .
C10 C9 1.393(3) .
C10 N4 1.402(3) .
C6 N4 1.368(3) .
C8 C9 1.388(4) .
C3 C2 1.391(4) .
