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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/4/35/04/4350481.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_4350481
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 Br0.92 I1.08 N4 O Zn'
_chemical_formula_weight         490.17
_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                 104.658(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0935(9)
_cell_length_b                   17.0287(16)
_cell_length_c                   8.5845(8)
_cell_measurement_temperature    173(2)
_cell_volume                     1427.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       8
_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            12474
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    6.628
_exptl_absorpt_correction_T_max  0.5293
_exptl_absorpt_correction_T_min  0.3109
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.282
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0278
_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)+(0.0049P)²+3.2227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                3411
_reflns_number_total             3560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060958gsi20060531_050744.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4350481
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
Br1 Br 0.86283(3) -0.507315(15) -0.28275(3) 0.03310(9) Uani 0.328(5) 1 d P
I1 I 0.86283(3) -0.507315(15) -0.28275(3) 0.03310(9) Uani 0.672(5) 1 d P
Br2 Br 0.53113(3) -0.337328(17) -0.40393(3) 0.03071(10) Uani 0.589(5) 1 d P
I2 I 0.53113(3) -0.337328(17) -0.40393(3) 0.03071(10) Uani 0.411(5) 1 d P
Zn1 Zn 0.73494(4) -0.39197(2) -0.21220(5) 0.02386(11) Uani 1 1 d .
O1 O 1.2777(2) -0.32916(14) -0.0765(3) 0.0257(5) Uani 1 1 d .
C6 C 1.2965(3) -0.32064(19) 0.0690(4) 0.0229(6) Uani 1 1 d .
N3 N 1.2100(3) -0.27712(17) 0.1366(3) 0.0254(6) Uani 1 1 d .
H3N H 1.2373 -0.2622 0.2378 0.030 Uiso 1 1 calc R
N1 N 0.8650(3) -0.30010(15) -0.1254(3) 0.0237(5) Uani 1 1 d .
N4 N 1.4018(3) -0.35401(18) 0.1817(3) 0.0277(6) Uani 1 1 d .
H4N H 1.4009 -0.3487 0.2834 0.033 Uiso 1 1 calc R
C10 C 1.5114(3) -0.39617(19) 0.1485(4) 0.0234(6) Uani 1 1 d .
C5 C 0.9921(3) -0.31517(19) -0.0377(4) 0.0240(6) Uani 1 1 d .
H5 H 1.0248 -0.3677 -0.0313 0.029 Uiso 1 1 calc R
C11 C 1.5619(3) -0.37991(19) 0.0157(4) 0.0245(6) Uani 1 1 d .
H11 H 1.5197 -0.3399 -0.0571 0.029 Uiso 1 1 calc R
C1 C 0.8190(4) -0.2258(2) -0.1338(4) 0.0316(7) Uani 1 1 d .
H1 H 0.7292 -0.2147 -0.1969 0.038 Uiso 1 1 calc R
C9 C 1.5733(3) -0.45514(19) 0.2539(4) 0.0270(7) Uani 1 1 d .
H9 H 1.5399 -0.4680 0.3447 0.032 Uiso 1 1 calc R
C2 C 0.8987(4) -0.1651(2) -0.0533(5) 0.0397(9) Uani 1 1 d .
H2 H 0.8636 -0.1131 -0.0609 0.048 Uiso 1 1 calc R
N2 N 1.6683(3) -0.41922(15) -0.0122(3) 0.0237(5) Uani 1 1 d .
C4 C 1.0781(3) -0.25644(18) 0.0445(4) 0.0223(6) Uani 1 1 d .
C7 C 1.7289(4) -0.4757(2) 0.0909(4) 0.0294(7) Uani 1 1 d .
H7 H 1.8048 -0.5031 0.0709 0.035 Uiso 1 1 calc R
C8 C 1.6840(4) -0.4947(2) 0.2249(4) 0.0314(7) Uani 1 1 d .
H8 H 1.7287 -0.5346 0.2965 0.038 Uiso 1 1 calc R
C3 C 1.0299(4) -0.1805(2) 0.0386(4) 0.0315(7) Uani 1 1 d .
H3 H 1.0854 -0.1397 0.0963 0.038 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'
Br Br -0.2901 2.4595 '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 100.56(11) 1_455 .
N2 Zn1 Br2 104.43(7) 1_455 .
N1 Zn1 Br2 107.62(8) . .
N2 Zn1 Br1 108.85(7) 1_455 .
N1 Zn1 Br1 111.28(8) . .
Br2 Zn1 Br1 121.825(18) . .
O1 C6 N4 124.4(3) . .
O1 C6 N3 122.8(3) . .
N4 C6 N3 112.8(3) . .
C6 N3 C4 120.4(3) . .
C5 N1 C1 118.7(3) . .
C5 N1 Zn1 119.4(2) . .
C1 N1 Zn1 121.1(2) . .
C6 N4 C10 125.4(3) . .
C11 C10 C9 118.7(3) . .
C11 C10 N4 122.4(3) . .
C9 C10 N4 119.0(3) . .
N1 C5 C4 122.2(3) . .
N2 C11 C10 121.7(3) . .
N1 C1 C2 121.9(3) . .
C8 C9 C10 119.1(3) . .
C1 C2 C3 119.7(3) . .
C11 N2 C7 119.5(3) . .
C11 N2 Zn1 119.0(2) . 1_655
C7 N2 Zn1 121.5(2) . 1_655
C3 C4 C5 119.1(3) . .
C3 C4 N3 122.0(3) . .
C5 C4 N3 118.9(3) . .
N2 C7 C8 121.8(3) . .
C7 C8 C9 119.2(3) . .
C4 C3 C2 118.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Zn1 2.5074(5) .
Br2 Zn1 2.4684(5) .
Zn1 N2 2.049(3) 1_455
Zn1 N1 2.057(3) .
O1 C6 1.224(4) .
C6 N4 1.367(4) .
C6 N3 1.380(4) .
N3 C4 1.410(4) .
N1 C5 1.338(4) .
N1 C1 1.343(4) .
N4 C10 1.407(4) .
C10 C11 1.389(5) .
C10 C9 1.390(4) .
C5 C4 1.393(4) .
C11 N2 1.338(4) .
C1 C2 1.382(5) .
C9 C8 1.380(5) .
C2 C3 1.384(5) .
N2 C7 1.344(4) .
N2 Zn1 2.049(3) 1_655
C4 C3 1.378(5) .
C7 C8 1.377(5) .
