#------------------------------------------------------------------------------
#$Date: 2015-10-06 16:05:13 +0300 (Tue, 06 Oct 2015) $
#$Revision: 160525 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/45/4124527.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_4124527
loop_
_publ_author_name
'Kwon, Hyuk Taek'
'Jeong, Hae-Kwon'
'Lee, Albert S.'
'An, He Seong'
'Lee, Jong Suk'
_publ_section_title
;
 Heteroepitaxially Grown Zeolitic Imidazolate Framework Membranes with
 Unprecedented Propylene/Propane Separation Performances.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12304
_journal_page_last               12311
_journal_paper_doi               10.1021/jacs.5b06730
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.08(C96 H120 N48 Zn12)'
_chemical_formula_sum            'C14 H24 N6 O2 Zn'
_chemical_formula_weight         373.76
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   16.8815(5)
_cell_length_b                   16.8815(5)
_cell_length_c                   16.8815(5)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    110
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      2.96
_cell_volume                     4811.0(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39822
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.520
_diffrn_reflns_theta_min         1.706
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1342 before and 0.0657 after correction.
The Ratio of minimum to maximum transmission is 0.7176.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.388
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
2 molecules of DMF (C3H7NO) per asymetric unit (24 per unit 
cell) were compensated for in the refinement.
TITL zif8_a.res in I-43m
CELL   16.8815   16.8815   16.8815     90.00     90.00     90.00
SPGR I-43m
C101 0.808 0.192 0.192 !       7.33 eA-3
C102 0.193 0.189 0.189 !       3.12 eA-3
C103 0.014 0.213 0.213 !       1.97 eA-3
C104 0.980 0.207 0.207 !       1.58 eA-3
C105 0.843 0.914 0.204 !       1.52 eA-3
C106 0.140 0.925 0.187 !       1.43 eA-3
C107 0.250 0.250 0.250 !       1.34 eA-3
C108 0.487 0.487 0.487 !       1.18 eA-3
C109 0.705 0.434 0.434 !       1.16 eA-3
C110 0.696 0.400 0.472 !       1.14 eA-3
C111 0.500 0.501 0.250 !       1.13 eA-3
C112 0.457 0.643 0.412 !       0.87 eA-3
C113 0.286 0.442 0.473 !       0.81 eA-3
C114 0.548 0.452 0.452 !       0.73 eA-3
C115 0.519 0.434 0.494 !       0.68 eA-3
C116 0.596 0.414 0.414 !       0.56 eA-3
C117 0.678 0.398 0.398 !       0.53 eA-3
C118 0.519 0.387 0.484 !       0.51 eA-3
;
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 588 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         1390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0275P)²+1.0144P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.829
_reflns_friedel_fraction_full    0.995
_reflns_friedel_fraction_max     0.997
_reflns_number_gt                1340
_reflns_number_total             1390
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b06730_si_002.cif
_cod_data_source_block           zif8_v_sq
_cod_depositor_comments
'Adding full bibliography for 4124527--4124528.cif.'
_cod_original_cell_volume        4811.0(4)
_cod_database_code               4124527
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.536
_platon_squeeze_void_probe_radius 1.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+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, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+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, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.2500 1.0000 0.02904(11) Uani 1 4 d S T P . .
C1 C 0.5047(3) 0.12374(8) 0.87626(8) 0.0283(4) Uani 1 2 d S T P . .
N1 N 0.46463(8) 0.18265(9) 0.91080(9) 0.0316(3) Uani 1 1 d . . . . .
C2 C 0.58565(15) 0.09766(13) 0.90234(13) 0.0372(5) Uani 1 2 d S T P . .
H2A H 0.6221 0.0995 0.8572 0.056 Uiso 0.5 1 calc GR . . A -1
H2B H 0.5829 0.0434 0.9227 0.056 Uiso 0.5 1 calc GR . . A -1
H2C H 0.6049 0.1331 0.9441 0.056 Uiso 0.5 1 calc GR . . A -1
C3 C 0.39263(11) 0.18517(13) 0.87171(12) 0.0401(4) Uani 1 1 d . . . . .
H3 H 0.3504 0.2207 0.8828 0.048 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'
Zn Zn 0.2839 1.4301 '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'
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 109.27(5) . 48_655
N1 Zn1 N1 109.27(5) . 46_456
N1 Zn1 N1 109.87(9) 48_655 46_456
N1 Zn1 N1 109.27(5) 48_655 3_657
N1 Zn1 N1 109.27(5) 3_657 46_456
N1 Zn1 N1 109.88(9) . 3_657
N1 C1 N1 113.2(3) 20_566 .
N1 C1 C2 123.41(16) 20_566 .
N1 C1 C2 123.41(16) . .
C1 N1 Zn1 127.35(17) . .
C1 N1 C3 105.0(2) . .
C3 N1 Zn1 127.61(12) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N1 C3 H3 125.8 . .
C3 C3 N1 108.39(10) 20_566 .
C3 C3 H3 125.8 20_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 1.9791(15) .
Zn1 N1 1.9791(15) 46_456
Zn1 N1 1.9791(15) 48_655
Zn1 N1 1.9791(15) 3_657
C1 N1 1.337(3) 20_566
C1 N1 1.337(3) .
C1 C2 1.502(5) .
N1 C3 1.384(2) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C3 1.358(4) 20_566
C3 H3 0.9500 .
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
Zn1 N1 C3 C3 -179.43(10) . 20_566
C1 N1 C3 C3 -0.61(18) . 20_566
N1 C1 N1 Zn1 179.87(8) 20_566 .
N1 C1 N1 C3 1.0(3) 20_566 .
C2 C1 N1 Zn1 1.3(4) . .
C2 C1 N1 C3 -177.5(2) . .
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
_platon_squeeze_void_content
1 -0.012 -0.006 -0.004 2317 773 ' '
