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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/77/1507799.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_1507799
loop_
_publ_author_name
'Tranchemontagne, David J.'
'Park, Kyo Sung'
'Furukawa, Hiroyasu'
'Eckert, Juergen'
'Knobler, Carolyn B.'
'Yaghi, Omar M.'
_publ_section_title
;
 Hydrogen Storage in New Metal--Organic Frameworks
;
_journal_issue                   24
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              13143
_journal_paper_doi               10.1021/jp302356q
_journal_volume                  116
_journal_year                    2012
_chemical_formula_moiety         'C48 H24 O13 Zn4'
_chemical_formula_sum            'C48 H24 O13 Zn4'
_chemical_formula_weight         1070.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           138
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2ac'
_symmetry_space_group_name_H-M   'P 42/n c m :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            4
_cell_length_a                   19.7213(13)
_cell_length_b                   19.7213(13)
_cell_length_c                   39.411(3)
_cell_measurement_reflns_used    1904
_cell_measurement_temperature    258(2)
_cell_measurement_theta_max      21.65
_cell_measurement_theta_min      2.31
_cell_volume                     15328.1(18)
_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      258(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS SMART APEX diffractometer'
_diffrn_measurement_method       'phi and 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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0256
_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       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            94159
_diffrn_reflns_theta_full        21.99
_diffrn_reflns_theta_max         21.99
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.9104
_exptl_absorpt_correction_T_min  0.7667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
' SADABS,  Ratio of minimum to maximum apparent transmission:  0.742373'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0955P)²+0.7228P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1554
_reflns_number_gt                3299
_reflns_number_total             4944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp302356q_si_002.cif
_cod_data_source_block           irmof-61
_cod_depositor_comments
'Adding full bibliography for 1507796--1507800.cif.'
_cod_original_cell_volume        15328.0(18)
_cod_original_sg_symbol_H-M      P4(2)/ncm
_cod_database_code               1507799
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z+1/2'
'y, -x+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'y+1/2, x+1/2, -z'
'-y, -x, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z-1/2'
'-y, x-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
'-y-1/2, -x-1/2, z'
'y, x, z'
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 0.306533(19) 0.193467(19) 0.324397(14) 0.0575(2) Uani 1 2 d S
Zn2 Zn 0.30702(2) 0.30702(2) 0.267452(14) 0.0623(2) Uani 1 2 d S
O1 O 0.2500 0.2500 0.29559(9) 0.0430(10) Uani 1 4 d S
O2 O 0.40107(14) 0.28923(17) 0.27559(9) 0.1122(11) Uani 1 1 d .
O3 O 0.40343(12) 0.20962(15) 0.31583(8) 0.0954(9) Uani 1 1 d .
O4 O 0.29014(17) 0.20986(17) 0.37228(10) 0.1040(14) Uani 1 2 d S
O5 O 0.28989(16) 0.21011(16) 0.72041(10) 0.1062(14) Uani 1 2 d S
C1 C 0.4314(2) 0.2505(2) 0.29509(12) 0.0927(14) Uani 1 1 d .
C2 C 0.50554(18) 0.2508(2) 0.29622(11) 0.0865(12) Uani 1 1 d .
C3 C 0.5412(2) 0.2929(3) 0.27533(17) 0.183(3) Uani 1 1 d .
H3 H 0.5180 0.3218 0.2607 0.219 Uiso 1 1 calc R
C4 C 0.6106(3) 0.2933(4) 0.27557(19) 0.198(4) Uani 1 1 d .
H4 H 0.6335 0.3234 0.2615 0.238 Uiso 1 1 calc R
C5 C 0.6468(2) 0.2514(3) 0.29554(14) 0.1156(17) Uani 1 1 d .
C6 C 0.6123(3) 0.2078(3) 0.31588(17) 0.161(3) Uani 1 1 d .
H6 H 0.6361 0.1776 0.3295 0.193 Uiso 1 1 calc R
C7 C 0.5413(2) 0.2079(3) 0.31650(16) 0.145(2) Uani 1 1 d .
H7 H 0.5184 0.1785 0.3309 0.174 Uiso 1 1 calc R
C8 C 0.7200(2) 0.2493(3) 0.29669(11) 0.1180(17) Uani 1 1 d .
C9 C 0.2500 0.2500 0.3875(2) 0.102(3) Uani 1 4 d S
C10 C 0.2500 0.2500 0.4234(2) 0.109(3) Uani 1 4 d S
C11 C 0.2914(4) 0.2086(4) 0.44097(18) 0.171(4) Uani 1 2 d S
H11 H 0.3205 0.1795 0.4295 0.205 Uiso 1 2 calc SR
C12 C 0.2907(4) 0.2093(4) 0.4769(2) 0.225(6) Uani 1 2 d S
H12 H 0.3198 0.1802 0.4884 0.269 Uiso 1 2 calc SR
C13 C 0.2500 0.2500 0.4951(3) 0.172(6) Uani 1 4 d S
C14 C 0.2500 0.2500 0.5315(3) 0.177(6) Uani 1 4 d S
C15 C 0.2500 0.2500 0.5608(3) 0.187(6) Uani 1 4 d S
C16 C 0.2500 0.2500 0.5985(3) 0.174(6) Uani 1 4 d S
C17 C 0.2928(3) 0.2072(3) 0.61492(18) 0.183(5) Uani 1 2 d S
H17 H 0.3216 0.1784 0.6030 0.219 Uiso 1 2 calc SR
C18 C 0.2919(3) 0.2081(3) 0.64959(16) 0.175(5) Uani 1 2 d S
H18 H 0.3208 0.1792 0.6614 0.210 Uiso 1 2 calc SR
C19 C 0.2500 0.2500 0.6675(2) 0.104(3) Uani 1 4 d S
C20 C 0.2500 0.2500 0.7065(2) 0.096(3) Uani 1 4 d S
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'
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 O1 112.14(16) . .
O4 Zn1 O3 107.56(12) . .
O1 Zn1 O3 111.36(10) . .
O4 Zn1 O3 107.56(12) . 15_665
O1 Zn1 O3 111.36(10) . 15_665
O3 Zn1 O3 106.58(17) . 15_665
O4 Zn1 Zn1 76.38(13) . 2
O1 Zn1 Zn1 35.76(9) . 2
O3 Zn1 Zn1 124.93(9) . 2
O3 Zn1 Zn1 124.93(9) 15_665 2
O5 Zn2 O2 107.50(12) 3_554 .
O5 Zn2 O2 107.50(12) 3_554 16
O2 Zn2 O2 109.1(2) . 16
O5 Zn2 O1 110.43(16) 3_554 .
O2 Zn2 O1 111.09(11) . .
O2 Zn2 O1 111.09(11) 16 .
Zn2 O1 Zn2 110.23(18) . 2
Zn2 O1 Zn1 109.524(12) . .
Zn2 O1 Zn1 109.525(12) 2 .
Zn2 O1 Zn1 109.522(12) . 2
Zn2 O1 Zn1 109.523(12) 2 2
Zn1 O1 Zn1 108.49(17) . 2
C1 O2 Zn2 133.2(3) . .
C1 O3 Zn1 129.3(3) . .
C9 O4 Zn1 131.9(5) . .
C20 O5 Zn2 130.8(5) . 4
O2 C1 O3 125.5(4) . .
O2 C1 C2 119.9(4) . .
O3 C1 C2 114.6(4) . .
C7 C2 C3 117.8(4) . .
C7 C2 C1 122.2(4) . .
C3 C2 C1 120.0(4) . .
C2 C3 C4 120.9(5) . .
C5 C4 C3 122.1(5) . .
C4 C5 C6 117.9(4) . .
C4 C5 C8 124.5(5) . .
C6 C5 C8 117.6(5) . .
C5 C6 C7 120.7(5) . .
C2 C7 C6 120.6(5) . .
C8 C8 C5 176.5(7) 2_655 .
O4 C9 O4 123.5(9) . 2
O4 C9 C10 118.3(4) . .
O4 C9 C10 118.3(4) 2 .
C11 C10 C11 118.1(9) . 2
C11 C10 C9 120.9(5) . .
C11 C10 C9 120.9(5) 2 .
C10 C11 C12 120.1(8) . .
C13 C12 C11 123.2(10) . .
C12 C13 C12 115.3(12) 2 .
C12 C13 C14 122.3(6) 2 .
C12 C13 C14 122.3(6) . .
C15 C14 C13 180.000(4) . .
C14 C15 C16 180.000(3) . .
C17 C16 C17 123.1(10) . 2
C17 C16 C15 118.5(5) . .
C17 C16 C15 118.5(5) 2 .
C16 C17 C18 117.5(9) . .
C17 C18 C19 122.1(8) . .
C18 C19 C18 117.9(9) . 2
C18 C19 C20 121.1(5) . .
C18 C19 C20 121.1(5) 2 .
O5 C20 O5 127.4(8) 2 .
O5 C20 C19 116.3(4) 2 .
O5 C20 C19 116.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.942(4) .
Zn1 O1 1.943(2) .
Zn1 O3 1.966(3) .
Zn1 O3 1.966(3) 15_665
Zn1 Zn1 3.1535(11) 2
Zn2 O5 1.915(4) 3_554
Zn2 O2 1.915(3) .
Zn2 O2 1.915(3) 16
Zn2 O1 1.939(2) .
O1 Zn2 1.939(2) 2
O1 Zn1 1.943(2) 2
O2 C1 1.238(4) .
O3 C1 1.273(4) .
O4 C9 1.271(5) .
O5 C20 1.241(5) .
O5 Zn2 1.914(4) 4
C1 C2 1.464(5) .
C2 C7 1.360(6) .
C2 C3 1.364(6) .
C3 C4 1.369(6) .
C4 C5 1.345(7) .
C5 C6 1.358(6) .
C5 C8 1.445(6) .
C6 C7 1.401(6) .
C8 C8 1.184(8) 2_655
C9 O4 1.271(5) 2
C9 C10 1.413(11) .
C10 C11 1.346(9) .
C10 C11 1.346(9) 2
C11 C12 1.414(11) .
C12 C13 1.342(10) .
C13 C12 1.342(10) 2
C13 C14 1.437(14) .
C14 C15 1.155(13) .
C15 C16 1.485(14) .
C16 C17 1.357(8) .
C16 C17 1.357(8) 2
C17 C18 1.367(9) .
C18 C19 1.365(8) .
C19 C18 1.365(8) 2
C19 C20 1.537(10) .
C20 O5 1.241(5) 2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O5 Zn2 O1 Zn2 0.0 3_554 2
O2 Zn2 O1 Zn2 -119.18(12) . 2
O2 Zn2 O1 Zn2 119.18(12) 16 2
O5 Zn2 O1 Zn1 120.57(11) 3_554 .
O2 Zn2 O1 Zn1 1.39(18) . .
O2 Zn2 O1 Zn1 -120.24(13) 16 .
O5 Zn2 O1 Zn1 -120.57(11) 3_554 2
O2 Zn2 O1 Zn1 120.25(13) . 2
O2 Zn2 O1 Zn1 -1.38(18) 16 2
O4 Zn1 O1 Zn2 119.50(11) . .
O3 Zn1 O1 Zn2 -1.09(16) . .
O3 Zn1 O1 Zn2 -119.91(12) 15_665 .
Zn1 Zn1 O1 Zn2 119.50(11) 2 .
O4 Zn1 O1 Zn2 -119.50(11) . 2
O3 Zn1 O1 Zn2 119.91(12) . 2
O3 Zn1 O1 Zn2 1.09(16) 15_665 2
Zn1 Zn1 O1 Zn2 -119.50(11) 2 2
O4 Zn1 O1 Zn1 0.0 . 2
O3 Zn1 O1 Zn1 -120.59(10) . 2
O3 Zn1 O1 Zn1 120.59(10) 15_665 2
O5 Zn2 O2 C1 -122.3(5) 3_554 .
O2 Zn2 O2 C1 121.4(4) 16 .
O1 Zn2 O2 C1 -1.4(5) . .
O4 Zn1 O3 C1 -122.8(4) . .
O1 Zn1 O3 C1 0.5(4) . .
O3 Zn1 O3 C1 122.1(4) 15_665 .
Zn1 Zn1 O3 C1 -37.4(4) 2 .
O1 Zn1 O4 C9 0.000(2) . .
O3 Zn1 O4 C9 122.77(10) . .
O3 Zn1 O4 C9 -122.77(10) 15_665 .
Zn1 Zn1 O4 C9 0.000(1) 2 .
Zn2 O2 C1 O3 0.7(8) . .
Zn2 O2 C1 C2 -177.4(3) . .
Zn1 O3 C1 O2 -0.1(7) . .
Zn1 O3 C1 C2 178.0(3) . .
O2 C1 C2 C7 -178.1(5) . .
O3 C1 C2 C7 3.6(7) . .
O2 C1 C2 C3 -1.2(8) . .
O3 C1 C2 C3 -179.5(5) . .
C7 C2 C3 C4 -1.9(10) . .
C1 C2 C3 C4 -178.9(6) . .
C2 C3 C4 C5 1.7(13) . .
C3 C4 C5 C6 0.1(11) . .
C3 C4 C5 C8 179.6(6) . .
C4 C5 C6 C7 -1.6(10) . .
C8 C5 C6 C7 178.9(5) . .
C3 C2 C7 C6 0.4(9) . .
C1 C2 C7 C6 177.4(5) . .
C5 C6 C7 C2 1.3(10) . .
C4 C5 C8 C8 12(8) . 2_655
C6 C5 C8 C8 -168(7) . 2_655
Zn1 O4 C9 O4 -0.001(3) . 2
Zn1 O4 C9 C10 180.000(1) . .
O4 C9 C10 C11 0.001(2) . .
O4 C9 C10 C11 180.002(2) 2 .
O4 C9 C10 C11 180.000(2) . 2
O4 C9 C10 C11 0.001(2) 2 2
C11 C10 C11 C12 0.003(4) 2 .
C9 C10 C11 C12 180.001(1) . .
C10 C11 C12 C13 -0.003(4) . .
C11 C12 C13 C12 0.000(5) . 2
C11 C12 C13 C14 180.001(4) . .
C12 C13 C14 C15 90(100) 2 .
C12 C13 C14 C15 -90(100) . .
C13 C14 C15 C16 0(100) . .
C14 C15 C16 C17 -90(100) . .
C14 C15 C16 C17 90(100) . 2
C17 C16 C17 C18 -0.003(4) 2 .
C15 C16 C17 C18 180.001(2) . .
C16 C17 C18 C19 -0.002(4) . .
C17 C18 C19 C18 0.000(4) . 2
C17 C18 C19 C20 180.001(3) . .
Zn2 O5 C20 O5 0.001(4) 4 2
Zn2 O5 C20 C19 179.999(2) 4 .
C18 C19 C20 O5 179.999(2) . 2
C18 C19 C20 O5 0.000(2) 2 2
C18 C19 C20 O5 0.000(2) . .
C18 C19 C20 O5 180.001(2) 2 .
