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#$Date: 2016-03-23 16:38:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179387 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/84/4328466.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_4328466
loop_
_publ_author_name
'Yan-Ping He'
'Yan-Xi Tan'
'Fei Wang'
'Jian Zhang'
_publ_contact_author_address
;
State Key Laboratory of Structural Chemistry, 
Fujian Institute of Research on the Structure of Matter, CAS
Fuzhou, Fujian, China 350002
;
_publ_contact_author_email       zhj@fjirsm.ac.cn
_publ_contact_author_name        'Jian Zhang'
_publ_contact_author_phone
;
;
_publ_section_title
;
 Microporous Zinc Tris[(4-carboxyl)phenylduryl]amine Framework with an
 Unusual Topological Net for Gas Storage and Separation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1995
_journal_page_last               1997
_journal_paper_doi               10.1021/ic202713e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C45 H38 N3 O9 Zn2'
_chemical_formula_weight         895.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_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            4
_cell_length_a                   11.9887(4)
_cell_length_b                   18.6365(4)
_cell_length_c                   17.9807(6)
_cell_measurement_reflns_used    827
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.18
_cell_volume                     4017.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8182
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3513
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0882P)²+3.7489P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                2691
_reflns_number_total             3513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202713e_si_002.cif
_cod_data_source_block           1
_cod_database_code               4328466
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, 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
Zn1 Zn 0.38961(4) 0.00896(3) 0.19757(3) 0.0237(2) Uani 1 1 d .
O4 O 0.2500 0.0000 0.1469(2) 0.0308(10) Uani 1 2 d S
C2 C 0.5985(4) -0.0524(2) 0.1507(2) 0.0300(10) Uani 1 1 d .
O3 O 0.5052(3) -0.02662(17) 0.13231(17) 0.0397(8) Uani 1 1 d .
C4 C 0.6627(4) -0.0901(2) 0.0924(2) 0.0303(10) Uani 1 1 d .
O2 O 0.9224(3) -0.88948(15) -0.21625(18) 0.0369(8) Uani 1 1 d .
C8 C 0.8839(4) -0.2215(3) -0.2073(3) 0.0417(13) Uani 1 1 d .
H8A H 0.8745 -0.2073 -0.2565 0.050 Uiso 1 1 calc R
O1 O 0.6403(3) -0.04902(18) 0.21451(17) 0.0390(8) Uani 1 1 d .
C10 C 0.9481(5) -0.2804(2) -0.1914(2) 0.0402(12) Uani 1 1 d .
C11 C 0.6196(4) -0.0971(3) 0.0216(3) 0.0403(12) Uani 1 1 d .
H11A H 0.5505 -0.0775 0.0101 0.048 Uiso 1 1 calc R
C12 C 0.9309(5) -0.7401(3) -0.2022(3) 0.0527(15) Uani 1 1 d .
H12A H 0.8836 -0.7646 -0.1701 0.063 Uiso 1 1 calc R
N1 N 1.0000 -0.3196(3) -0.2500 0.0476(16) Uani 1 2 d S
C14 C 1.0000 -0.3959(3) -0.2500 0.0398(17) Uani 1 2 d S
C15 C 0.6797(4) -0.1337(3) -0.0322(3) 0.0438(12) Uani 1 1 d .
H15A H 0.6494 -0.1386 -0.0795 0.053 Uiso 1 1 calc R
C16 C 1.0000 -0.6268(3) -0.2500 0.0416(17) Uani 1 2 d S
C17 C 1.0000 -0.8588(3) -0.2500 0.0241(13) Uani 1 2 d S
C18 C 1.0000 -0.5471(3) -0.2500 0.0431(17) Uani 1 2 d S
C19 C 0.7836(4) -0.1632(2) -0.0177(3) 0.0394(11) Uani 1 1 d .
C20 C 0.8450(4) -0.2023(2) -0.0767(3) 0.0404(12) Uani 1 1 d .
C21 C 0.9320(5) -0.6659(3) -0.2021(3) 0.0570(16) Uani 1 1 d .
H21A H 0.8860 -0.6414 -0.1691 0.068 Uiso 1 1 calc R
C22 C 0.9145(5) -0.4340(3) -0.2177(3) 0.0543(16) Uani 1 1 d .
H22A H 0.8550 -0.4097 -0.1961 0.065 Uiso 1 1 calc R
C23 C 0.8265(5) -0.1549(3) 0.0535(3) 0.0523(14) Uani 1 1 d .
H23A H 0.8965 -0.1734 0.0649 0.063 Uiso 1 1 calc R
C24 C 1.0000 -0.7782(3) -0.2500 0.0311(14) Uani 1 2 d S
C25 C 0.7662(4) -0.1195(3) 0.1076(3) 0.0442(13) Uani 1 1 d .
H25A H 0.7958 -0.1153 0.1552 0.053 Uiso 1 1 calc R
C26 C 0.8330(4) -0.1830(2) -0.1511(3) 0.0402(12) Uani 1 1 d .
H26A H 0.7896 -0.1433 -0.1632 0.048 Uiso 1 1 calc R
C27 C 0.9166(5) -0.5079(3) -0.2173(4) 0.0542(16) Uani 1 1 d .
H27A H 0.8589 -0.5323 -0.1937 0.065 Uiso 1 1 calc R
C28 C 0.9640(5) -0.2998(3) -0.1178(3) 0.0572(16) Uani 1 1 d .
H28A H 1.0086 -0.3391 -0.1063 0.069 Uiso 1 1 calc R
C29 C 0.9133(5) -0.2606(3) -0.0607(3) 0.0567(16) Uani 1 1 d .
H29A H 0.9255 -0.2737 -0.0114 0.068 Uiso 1 1 calc R
N2 N 0.7898(12) -0.3933(8) 0.0518(7) 0.191(5) Uiso 1 1 d D
O5 O 0.7199(14) -0.4133(11) -0.0600(9) 0.323(9) Uiso 1 1 d D
C32 C 0.6963(17) -0.3692(10) -0.0098(11) 0.231(7) Uiso 1 1 d D
H32A H 0.6421 -0.3335 -0.0081 0.277 Uiso 1 1 calc R
C31 C 0.8861(15) -0.4462(15) 0.0486(12) 0.284(11) Uiso 1 1 d .
H31A H 0.8850 -0.4709 0.0018 0.426 Uiso 1 1 calc R
H31B H 0.8788 -0.4804 0.0883 0.426 Uiso 1 1 calc R
H31C H 0.9553 -0.4208 0.0538 0.426 Uiso 1 1 calc R
C30 C 0.7678(14) -0.3417(10) 0.1132(11) 0.232(8) Uiso 1 1 d .
H30A H 0.8205 -0.3494 0.1526 0.349 Uiso 1 1 calc R
H30B H 0.6935 -0.3489 0.1318 0.349 Uiso 1 1 calc R
H30C H 0.7750 -0.2936 0.0949 0.349 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'
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
O4 Zn1 O3 107.92(14) . .
O4 Zn1 O1 100.22(13) . 3_655
O3 Zn1 O1 115.74(14) . 3_655
O4 Zn1 O2 109.93(10) . 6_565
O3 Zn1 O2 106.94(14) . 6_565
O1 Zn1 O2 115.66(14) 3_655 6_565
Zn1 O4 Zn1 123.1(2) . 2
O1 C2 O3 125.1(4) . .
O1 C2 C4 117.7(4) . .
O3 C2 C4 117.2(4) . .
C2 O3 Zn1 127.4(3) . .
C11 C4 C25 118.6(4) . .
C11 C4 C2 120.4(4) . .
C25 C4 C2 121.0(4) . .
C17 O2 Zn1 132.4(3) . 6_645
C10 C8 C26 120.7(4) . .
C10 C8 H8A 119.7 . .
C26 C8 H8A 119.7 . .
C2 O1 Zn1 134.2(3) . 3_655
C8 C10 C28 119.1(4) . .
C8 C10 N1 120.1(4) . .
C28 C10 N1 120.9(4) . .
C4 C11 C15 119.8(4) . .
C4 C11 H11A 120.1 . .
C15 C11 H11A 120.1 . .
C21 C12 C24 120.4(5) . .
C21 C12 H12A 119.8 . .
C24 C12 H12A 119.8 . .
C14 N1 C10 120.8(2) . 3_754
C14 N1 C10 120.8(2) . .
C10 N1 C10 118.3(5) 3_754 .
C22 C14 C22 117.8(6) . 3_754
C22 C14 N1 121.1(3) . .
C22 C14 N1 121.1(3) 3_754 .
C11 C15 C19 122.1(5) . .
C11 C15 H15A 119.0 . .
C19 C15 H15A 119.0 . .
C21 C16 C21 116.9(6) . 3_754
C21 C16 C18 121.6(3) . .
C21 C16 C18 121.6(3) 3_754 .
O2 C17 O2 125.5(5) . 3_754
O2 C17 C24 117.2(3) . .
O2 C17 C24 117.2(3) 3_754 .
C27 C18 C27 115.6(6) 3_754 .
C27 C18 C16 122.2(3) 3_754 .
C27 C18 C16 122.2(3) . .
C15 C19 C23 117.4(4) . .
C15 C19 C20 120.5(4) . .
C23 C19 C20 122.1(5) . .
C29 C20 C26 117.4(4) . .
C29 C20 C19 121.9(4) . .
C26 C20 C19 120.6(4) . .
C12 C21 C16 121.9(5) . .
C12 C21 H21A 119.1 . .
C16 C21 H21A 119.1 . .
C14 C22 C27 120.3(5) . .
C14 C22 H22A 119.8 . .
C27 C22 H22A 119.8 . .
C25 C23 C19 120.7(5) . .
C25 C23 H23A 119.7 . .
C19 C23 H23A 119.7 . .
C12 C24 C12 118.5(6) 3_754 .
C12 C24 C17 120.8(3) 3_754 .
C12 C24 C17 120.8(3) . .
C23 C25 C4 121.3(4) . .
C23 C25 H25A 119.3 . .
C4 C25 H25A 119.3 . .
C8 C26 C20 121.6(5) . .
C8 C26 H26A 119.2 . .
C20 C26 H26A 119.2 . .
C18 C27 C22 122.9(5) . .
C18 C27 H27A 118.5 . .
C22 C27 H27A 118.5 . .
C10 C28 C29 120.4(5) . .
C10 C28 H28A 119.8 . .
C29 C28 H28A 119.8 . .
C20 C29 C28 120.8(5) . .
C20 C29 H29A 119.6 . .
C28 C29 H29A 119.6 . .
C30 N2 C31 125.6(15) . .
C30 N2 C32 101.7(14) . .
C31 N2 C32 132.2(14) . .
O5 C32 N2 98.8(15) . .
O5 C32 H32A 130.6 . .
N2 C32 H32A 130.6 . .
N2 C31 H31A 109.5 . .
N2 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
N2 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
N2 C30 H30A 109.5 . .
N2 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
N2 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.913(2) .
Zn1 O3 1.933(3) .
Zn1 O1 1.948(3) 3_655
Zn1 O2 1.962(3) 6_565
O4 Zn1 1.913(2) 2
C2 O1 1.253(5) .
C2 O3 1.262(5) .
C2 C4 1.477(6) .
C4 C11 1.380(7) .
C4 C25 1.384(6) .
O2 C17 1.250(4) .
O2 Zn1 1.962(3) 6_645
C8 C10 1.371(7) .
C8 C26 1.382(6) .
C8 H8A 0.9300 .
O1 Zn1 1.948(3) 3_655
C10 C28 1.384(7) .
C10 N1 1.425(5) .
C11 C15 1.385(7) .
C11 H11A 0.9300 .
C12 C21 1.383(7) .
C12 C24 1.388(6) .
C12 H12A 0.9300 .
N1 C14 1.422(8) .
N1 C10 1.425(5) 3_754
C14 C22 1.375(6) .
C14 C22 1.375(6) 3_754
C15 C19 1.387(7) .
C15 H15A 0.9300 .
C16 C21 1.391(6) .
C16 C21 1.391(6) 3_754
C16 C18 1.485(8) .
C17 O2 1.250(4) 3_754
C17 C24 1.502(7) .
C18 C27 1.371(6) 3_754
C18 C27 1.371(6) .
C19 C23 1.389(7) .
C19 C20 1.481(6) .
C20 C29 1.391(7) .
C20 C26 1.393(7) .
C21 H21A 0.9300 .
C22 C27 1.378(7) .
C22 H22A 0.9300 .
C23 C25 1.379(7) .
C23 H23A 0.9300 .
C24 C12 1.388(6) 3_754
C25 H25A 0.9300 .
C26 H26A 0.9300 .
C27 H27A 0.9300 .
C28 C29 1.399(7) .
C28 H28A 0.9300 .
C29 H29A 0.9300 .
N2 C30 1.488(19) .
N2 C31 1.52(2) .
N2 C32 1.640(15) .
O5 C32 1.25(2) .
C32 H32A 0.9300 .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 0.9600 .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
