#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:30:31 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179582 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/47/4504743.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_4504743
loop_
_publ_author_name
'Custelcean, Radu'
'Moyer, Bruce A.'
'Bryantsev, Vyacheslav S.'
'Hay, Benjamin P.'
_publ_section_title
;
 Anion Coordination in Metal−Organic Frameworks Functionalized with
 Urea Hydrogen-Bonding Groups
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              555
_journal_paper_doi               10.1021/cg0505057
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C22 H20 Cl2 N8 O10 Zn'
_chemical_formula_weight         692.73
_chemical_name_common            5
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :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            8
_cell_length_a                   16.9462(15)
_cell_length_b                   16.9462(15)
_cell_length_c                   18.477(3)
_cell_measurement_temperature    173(2)
_cell_volume                     5306.1(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0217
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32769
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  0.9314
_exptl_absorpt_correction_T_min  0.7072
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.381
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.381
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0632
_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)+(0.0369P)²+27.8101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                3200
_reflns_number_total             3304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0505057si20050928_052814.cif
_cod_data_source_block           c:\frames\075\work\075s
_cod_original_cell_volume        5306.0(12)
_cod_original_sg_symbol_H-M      I41/a
_cod_database_code               4504743
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'
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 0.0000 0.7500 0.11410(3) 0.01537(16) Uani 1 2 d S
Cl1 Cl 0.25394(5) 0.74514(5) 0.00725(4) 0.0231(2) Uani 1 1 d .
N1 N -0.02708(17) 0.65822(17) 0.05029(15) 0.0174(6) Uani 1 1 d .
N3 N 0.09065(17) 0.72906(17) 0.18168(15) 0.0174(6) Uani 1 1 d .
O1 O 0.25354(15) 0.50890(15) 0.30610(13) 0.0220(5) Uani 1 1 d .
N4 N 0.23071(18) 0.56806(18) 0.19649(15) 0.0202(6) Uani 1 1 d .
H4N H 0.2452 0.5658 0.1508 0.024 Uiso 1 1 calc R
C10 C 0.1363(2) 0.6663(2) 0.16817(18) 0.0177(6) Uani 1 1 d .
H10 H 0.1328 0.6421 0.1219 0.021 Uiso 1 1 calc R
C9 C 0.1884(2) 0.6351(2) 0.21830(18) 0.0172(6) Uani 1 1 d .
N2 N -0.18995(18) 0.51911(18) 0.04937(15) 0.0207(6) Uani 1 1 d .
H2N H -0.1884 0.5037 0.0948 0.025 Uiso 1 1 calc R
C7 C 0.1473(2) 0.7370(2) 0.2994(2) 0.0241(7) Uani 1 1 d .
H7 H 0.1504 0.7629 0.3449 0.029 Uiso 1 1 calc R
C5 C -0.0902(2) 0.6156(2) 0.06854(17) 0.0169(6) Uani 1 1 d .
H5 H -0.1130 0.6234 0.1149 0.020 Uiso 1 1 calc R
C4 C -0.1240(2) 0.5601(2) 0.02250(17) 0.0171(6) Uani 1 1 d .
C8 C 0.1936(2) 0.6709(2) 0.28585(18) 0.0214(7) Uani 1 1 d .
H8 H 0.2281 0.6507 0.3219 0.026 Uiso 1 1 calc R
C2 C -0.0250(2) 0.5936(2) -0.0641(2) 0.0264(8) Uani 1 1 d .
H2 H -0.0011 0.5867 -0.1102 0.032 Uiso 1 1 calc R
C3 C -0.0910(2) 0.5492(2) -0.04525(19) 0.0234(7) Uani 1 1 d .
H3 H -0.1130 0.5122 -0.0782 0.028 Uiso 1 1 calc R
O3 O 0.2943(2) 0.7407(2) -0.06031(17) 0.0472(9) Uani 1 1 d .
C1 C 0.0054(2) 0.6474(2) -0.0159(2) 0.0225(7) Uani 1 1 d .
H1 H 0.0502 0.6778 -0.0294 0.027 Uiso 1 1 calc R
C11 C 0.25143(19) 0.5061(2) 0.23948(17) 0.0158(6) Uani 1 1 d .
C6 C 0.0969(2) 0.7647(2) 0.24709(19) 0.0213(7) Uani 1 1 d .
H6 H 0.0657 0.8101 0.2569 0.026 Uiso 1 1 calc R
O4 O 0.2758(2) 0.6782(2) 0.05201(18) 0.0430(8) Uani 1 1 d .
O2 O 0.17013(18) 0.7430(2) -0.00447(19) 0.0453(9) Uani 1 1 d .
O5 O 0.2742(2) 0.8164(2) 0.0444(2) 0.0467(9) Uani 1 1 d .
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'
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'
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 Zn1 N1 107.97(17) 3_565 .
N1 Zn1 N3 109.10(11) 3_565 .
N1 Zn1 N3 113.76(11) . .
N1 Zn1 N3 113.76(11) 3_565 3_565
N1 Zn1 N3 109.10(11) . 3_565
N3 Zn1 N3 103.24(16) . 3_565
O3 Cl1 O5 110.4(2) . .
O3 Cl1 O2 110.0(2) . .
O5 Cl1 O2 109.3(2) . .
O3 Cl1 O4 109.6(2) . .
O5 Cl1 O4 109.0(2) . .
O2 Cl1 O4 108.6(2) . .
C5 N1 C1 118.8(3) . .
C5 N1 Zn1 117.1(2) . .
C1 N1 Zn1 122.9(2) . .
C10 N3 C6 118.4(3) . .
C10 N3 Zn1 117.8(2) . .
C6 N3 Zn1 122.3(2) . .
C11 N4 C9 126.0(3) . .
N3 C10 C9 123.2(3) . .
C10 C9 C8 118.3(3) . .
C10 C9 N4 116.3(3) . .
C8 C9 N4 125.3(3) . .
C11 N2 C4 125.1(3) 16 .
C6 C7 C8 120.0(3) . .
N1 C5 C4 122.8(3) . .
C3 C4 C5 118.4(3) . .
C3 C4 N2 125.1(3) . .
C5 C4 N2 116.4(3) . .
C9 C8 C7 118.5(3) . .
C1 C2 C3 119.8(3) . .
C4 C3 C2 118.6(3) . .
N1 C1 C2 121.5(3) . .
O1 C11 N4 124.1(3) . .
O1 C11 N2 123.4(3) . 14
N4 C11 N2 112.5(3) . 14
N3 C6 C7 121.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.005(3) 3_565
Zn1 N1 2.005(3) .
Zn1 N3 2.011(3) .
Zn1 N3 2.011(3) 3_565
Cl1 O3 1.426(3) .
Cl1 O5 1.431(3) .
Cl1 O2 1.437(3) .
Cl1 O4 1.452(3) .
N1 C5 1.334(4) .
N1 C1 1.354(4) .
N3 C10 1.338(4) .
N3 C6 1.356(4) .
O1 C11 1.232(4) .
N4 C11 1.362(4) .
N4 C9 1.403(4) .
C10 C9 1.384(5) .
C9 C8 1.391(5) .
N2 C11 1.365(4) 16
N2 C4 1.406(4) .
C7 C6 1.373(5) .
C7 C8 1.391(5) .
C5 C4 1.392(4) .
C4 C3 1.383(5) .
C2 C1 1.376(5) .
C2 C3 1.392(5) .
C11 N2 1.365(4) 14
