#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/06/7200658.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_7200658
loop_
_publ_author_name
'Choi, Eun-Young'
'Wray, Curtis A.'
'Hu, Chunhua'
'Choe, Wonyoung'
_publ_section_title
;
 Highly tunable metal--organic frameworks with open metal centers
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              553
_journal_paper_doi               10.1039/b819707p
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C48 H30 N4 O11 Zn3'
_chemical_formula_sum            'C48 H30 N4 O11 Zn3'
_chemical_formula_weight         1034.87
_chemical_name_systematic
;
?
;
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.6814(10)
_cell_length_b                   16.6814(10)
_cell_length_c                   17.4944(15)
_cell_measurement_reflns_used    6453
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.33
_cell_volume                     4868.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'omega 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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26855
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.9701
_exptl_absorpt_correction_T_min  0.8439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       star-shape
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
Disordered, independent solvent molecules were eliminated from the refinement
using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13].

R factors before data are squeezed:
_refine_ls_R_factor_all 0.1151
_refine_ls_R_factor_gt 0.1081
_refine_ls_wR_factor_ref 0.3412
_refine_ls_wR_factor_gt 0.3324
;
_refine_diff_density_max         2.262
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1393
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0629
_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)+(0.1370P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1713
_refine_ls_wR_factor_ref         0.1743
_reflns_number_gt                1287
_reflns_number_total             1393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b819707p.txt
_cod_data_source_block           c7ch30-i4mmmsq
_cod_original_sg_symbol_Hall     '-I 4 2 '
_cod_database_code               7200658
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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 0.5000 0.5000 0.98061(6) 0.0314(5) Uani 0.50 8 d SP . .
Zn2 Zn 0.0000 0.0000 1.08218(4) 0.0352(3) Uani 1 8 d S . .
O1 O 0.08470(9) 0.08470(9) 1.06343(16) 0.0685(8) Uani 1 2 d S . .
N1 N 0.37777(18) 0.5000 1.0000 0.0429(8) Uani 1 4 d S . .
C1 C 0.32863(16) 0.43400(16) 1.0000 0.0467(8) Uani 1 2 d S . .
C2 C 0.24608(16) 0.45999(19) 1.0000 0.0579(9) Uani 1 2 d S . .
H2 H 0.2002 0.4263 1.0000 0.069 Uiso 1 2 calc SR . .
C3 C 0.35445(16) 0.35445(16) 1.0000 0.0488(10) Uani 1 4 d S . .
C4 C 0.29066(17) 0.29066(17) 1.0000 0.0479(11) Uani 1 4 d S . .
C5 C 0.2487(3) 0.2730(3) 1.0663(3) 0.056(2) Uani 0.50 1 d P . .
H5 H 0.2601 0.3013 1.1122 0.068 Uiso 0.50 1 calc PR . .
C6 C 0.1902(3) 0.2139(4) 1.0658(3) 0.059(2) Uani 0.50 1 d P . .
H6 H 0.1620 0.2020 1.1115 0.070 Uiso 0.50 1 calc PR . .
C7 C 0.17236(15) 0.17236(15) 1.0000 0.0451(10) Uani 1 4 d S . .
C8 C 0.10882(16) 0.10882(16) 1.0000 0.0458(10) Uani 1 4 d S . .
O2 O 0.5000 0.5000 0.8572(5) 0.0448(19) Uani 0.50 8 d SPD . .
H2O H 0.5361(8) 0.5361(8) 0.8370(7) 0.054 Uiso 0.25 2 d SPRD . .
O3 O 0.0000 0.0000 1.1962(3) 0.0718(18) Uani 1 8 d SD . .
H3O H 0.0000 0.0489 1.2210 0.086 Uiso 0.50 2 d SPRD . .
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
_geom_angle_publ_flag
N1 Zn1 N1 88.456(11) 19_567 17_667 ?
N1 Zn1 N1 161.11(6) 19_567 3_655 ?
N1 Zn1 N1 88.456(11) 17_667 3_655 ?
N1 Zn1 N1 88.456(11) 19_567 . ?
N1 Zn1 N1 161.11(6) 17_667 . ?
N1 Zn1 N1 88.456(11) 3_655 . ?
N1 Zn1 O2 99.45(3) 19_567 . ?
N1 Zn1 O2 99.45(3) 17_667 . ?
N1 Zn1 O2 99.45(3) 3_655 . ?
N1 Zn1 O2 99.45(3) . . ?
O3 Zn2 O1 99.32(8) . 2 ?
O3 Zn2 O1 99.32(8) . 3 ?
O1 Zn2 O1 88.50(3) 2 3 ?
O3 Zn2 O1 99.32(8) . . ?
O1 Zn2 O1 161.35(16) 2 . ?
O1 Zn2 O1 88.50(3) 3 . ?
O3 Zn2 O1 99.32(8) . 4 ?
O1 Zn2 O1 88.50(3) 2 4 ?
O1 Zn2 O1 161.35(16) 3 4 ?
O1 Zn2 O1 88.50(3) . 4 ?
O3 Zn2 Zn2 180.000(1) . 17_557 ?
O1 Zn2 Zn2 80.68(8) 2 17_557 ?
O1 Zn2 Zn2 80.68(8) 3 17_557 ?
O1 Zn2 Zn2 80.68(8) . 17_557 ?
O1 Zn2 Zn2 80.68(8) 4 17_557 ?
C8 O1 Zn2 126.5(2) . . ?
C1 N1 C1 106.7(3) . 21_565 ?
C1 N1 Zn1 126.09(14) . 17_667 ?
C1 N1 Zn1 126.09(14) 21_565 17_667 ?
C1 N1 Zn1 126.09(14) . . ?
C1 N1 Zn1 126.09(14) 21_565 . ?
N1 C1 C3 125.4(3) . . ?
N1 C1 C2 109.2(2) . . ?
C3 C1 C2 125.5(3) . . ?
C2 C2 C1 107.48(17) 21_565 . ?
C2 C2 H2 126.3 21_565 . ?
C1 C2 H2 126.3 . . ?
C1 C3 C1 126.0(4) 7_557 . ?
C1 C3 C4 117.02(18) 7_557 . ?
C1 C3 C4 117.02(18) . . ?
C5 C4 C5 119.1(5) 7_557 . ?
C5 C4 C5 113.6(5) 18_557 . ?
C5 C4 C5 113.6(5) 7_557 24 ?
C5 C4 C5 119.1(5) 18_557 24 ?
C5 C4 C3 120.5(2) 7_557 . ?
C5 C4 C3 120.5(2) 18_557 . ?
C5 C4 C3 120.5(2) . . ?
C5 C4 C3 120.5(2) 24 . ?
C4 C5 C6 120.0(5) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 121.1(4) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C6 118.8(5) 24 18_557 ?
C6 C7 C6 113.5(5) . 18_557 ?
C6 C7 C6 113.5(5) 24 7_557 ?
C6 C7 C6 118.8(5) . 7_557 ?
C6 C7 C8 120.6(2) 24 . ?
C6 C7 C8 120.6(2) . . ?
C6 C7 C8 120.6(2) 18_557 . ?
C6 C7 C8 120.6(2) 7_557 . ?
O1 C8 O1 125.7(4) 18_557 . ?
O1 C8 C7 117.15(19) 18_557 . ?
O1 C8 C7 117.15(19) . . ?
Zn1 O2 H2O 112.6 . . ?
Zn2 O3 H3O 118.0 . . ?
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 N1 2.067(3) . ?
Zn1 O2 2.158(9) . ?
Zn2 O3 1.995(5) . ?
Zn2 O1 2.025(2) . ?
Zn2 Zn2 2.8755(13) 17_557 ?
O1 C8 1.247(3) . ?
N1 C1 1.373(3) . ?
N1 Zn1 2.067(3) 17_667 ?
C1 C3 1.395(3) . ?
C1 C2 1.444(4) . ?
C2 C2 1.335(6) 21_565 ?
C2 H2 0.9500 . ?
C3 C4 1.505(5) . ?
C4 C5 1.387(5) . ?
C4 C5 1.387(5) 24 ?
C5 C6 1.388(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(5) . ?
C6 H6 0.9500 . ?
C7 C6 1.376(5) 24 ?
C7 C8 1.499(5) . ?
O2 H2O 0.9224 . ?
O3 H3O 0.9233 . ?
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 -0.036 0.250 0.215 3155.9 739.3
