#------------------------------------------------------------------------------
#$Date: 2019-11-25 04:51:04 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240048 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/93/4129302.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_4129302
loop_
_publ_author_name
'Liu, Lujia'
'Telfer, Shane G.'
_publ_section_title
;
 Systematic ligand modulation enhances the moisture stability and gas
 sorption characteristics of quaternary metal-organic frameworks.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3901
_journal_page_last               3909
_journal_paper_doi               10.1021/jacs.5b00365
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C115 H154 O13 Zn4'
_chemical_formula_weight         2005.85
_space_group_crystal_system      cubic
_space_group_IT_number           200
_space_group_name_Hall           '-P 2 2 3'
_space_group_name_H-M_alt        'P m -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   29.8116(15)
_cell_length_b                   29.8116(15)
_cell_length_c                   29.8116(15)
_cell_measurement_reflns_used    22099
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      58.97
_cell_measurement_theta_min      6.64
_cell_volume                     26495(2)
_computing_cell_refinement       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_molecular_graphics    'OLEX (Dolomanov, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.795
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.795
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65369
_diffrn_reflns_point_group_measured_fraction_full 0.795
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.922
_diffrn_reflns_theta_min         6.641
_diffrn_source                   'Rigaku MM007 rotating anode'
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.365499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6408
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.458
_exptl_crystal_size_min          0.452
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         6768
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0803
_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)+(0.1761P)²+4.6983P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2579
_refine_ls_wR_factor_ref         0.2756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5139
_reflns_number_total             6768
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b00365_si_002.cif
_cod_data_source_block           MUF-77-Octyl
_cod_original_cell_volume        26495(4)
_cod_database_code               4129302
_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_min   0.663
_shelx_estimated_absorpt_t_max   0.688
_shelxl_version_number           2013-2
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'
'-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'
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
Zn1 Zn 0.44648(2) 0.32283(2) 0.0000 0.0811(3) Uani 1 2 d S T P
Zn2 Zn 0.5000 0.24863(2) 0.05292(2) 0.0841(3) Uani 1 2 d S T P
O1 O 0.5000 0.28605(12) 0.0000 0.0708(11) Uani 1 4 d S T P
O2 O 0.46307(16) 0.38499(13) 0.0000 0.1206(15) Uani 1 2 d S T P
O5 O 0.44743(12) 0.25908(12) 0.08882(12) 0.1284(12) Uani 1 1 d . . .
O4 O 0.41015(12) 0.31273(12) 0.05171(12) 0.1257(11) Uani 1 1 d . . .
O3 O 0.5000 0.18652(15) 0.03747(19) 0.1439(19) Uani 1 2 d S T P
C1 C 0.5000 0.4043(3) 0.0000 0.104(3) Uani 1 4 d S T P
C2 C 0.5000 0.4532(3) 0.0000 0.105(3) Uani 1 4 d S T P
C9 C 0.41513(18) 0.28644(19) 0.08347(19) 0.1211(16) Uani 1 1 d . . .
C4 C 0.5000 0.1677(3) 0.0000 0.132(4) Uani 1 4 d S T P
C13 C 0.3126(2) 0.2859(2) 0.1823(2) 0.178(3) Uani 1 1 d . . .
C3 C 0.4603(3) 0.4769(2) 0.0000 0.142(3) Uani 1 2 d S T P
H3 H 0.4331 0.4615 0.0000 0.170 Uiso 1 2 calc R U P
C14 C 0.3455(2) 0.2539(2) 0.1844(2) 0.160(3) Uani 1 1 d . . .
C5 C 0.5000 0.1177(3) 0.0000 0.177(6) Uani 1 4 d S T P
C15 C 0.3807(2) 0.2540(2) 0.1511(2) 0.161(3) Uani 1 1 d . . .
H15 H 0.4037 0.2329 0.1519 0.193 Uiso 1 1 calc R U .
C10 C 0.3792(2) 0.2859(2) 0.1186(2) 0.152(2) Uani 1 1 d . . .
C11 C 0.3451(2) 0.3179(2) 0.1173(2) 0.185(3) Uani 1 1 d . . .
H11 H 0.3448 0.3393 0.0945 0.222 Uiso 1 1 calc R U .
C8 C 0.5000 0.0238(4) 0.0000 0.223(9) Uani 1 4 d S T P
C6 C 0.5000 0.0942(3) 0.0392(4) 0.264(8) Uani 1 2 d S T P
H6 H 0.5000 0.1091 0.0666 0.317 Uiso 1 2 calc R U P
C18 C 0.3409(3) 0.2206(3) 0.2212(3) 0.176(3) Uani 1 1 d . . .
C16 C 0.2812(2) 0.2773(3) 0.2228(2) 0.176(3) Uani 1 1 d . . .
C12 C 0.3119(3) 0.3184(3) 0.1493(3) 0.221(5) Uani 1 1 d . . .
H12 H 0.2894 0.3400 0.1487 0.265 Uiso 1 1 calc R U .
C17 C 0.2981(2) 0.2388(2) 0.2441(2) 0.169(3) Uani 1 1 d . . .
C7 C 0.5000 0.0483(3) 0.0373(4) 0.272(9) Uani 1 2 d S T P
H7 H 0.5000 0.0329 0.0644 0.327 Uiso 1 2 calc R U P
C22 C 0.3832(3) 0.2240(4) 0.2530(3) 0.245(6) Uani 1 1 d . . .
H22A H 0.4100 0.2158 0.2364 0.295 Uiso 1 1 calc R U .
H22B H 0.3799 0.2032 0.2778 0.295 Uiso 1 1 calc R U .
C19 C 0.3339(4) 0.1741(3) 0.2003(4) 0.229(5) Uani 1 1 d . . .
H19A H 0.3610 0.1659 0.1843 0.275 Uiso 1 1 calc R U .
H19B H 0.3300 0.1526 0.2244 0.275 Uiso 1 1 calc R U .
C20 C 0.2946(5) 0.1696(6) 0.1685(5) 0.326(8) Uiso 1 1 d D . .
H20A H 0.2970 0.1929 0.1459 0.392 Uiso 1 1 calc R U .
H20B H 0.2672 0.1749 0.1852 0.392 Uiso 1 1 calc R U .
C21 C 0.2903(6) 0.1222(5) 0.1435(6) 0.392 Uiso 1 1 d D U .
H21A H 0.2643 0.1224 0.1245 0.489 Uiso 1 1 calc R U .
H21B H 0.2875 0.0988 0.1654 0.489 Uiso 1 1 calc R U .
H21C H 0.3166 0.1171 0.1256 0.489 Uiso 1 1 calc R U .
C23 C 0.3883(6) 0.2767(6) 0.2727(6) 0.355(9) Uiso 1 1 d D . .
H23A H 0.3935 0.2981 0.2488 0.425 Uiso 1 1 calc R U .
H23B H 0.3623 0.2857 0.2901 0.425 Uiso 1 1 calc R U .
C24 C 0.4306(7) 0.2703(6) 0.3028(6) 0.425 Uiso 1 1 d D U .
H24A H 0.4379 0.2982 0.3171 0.532 Uiso 1 1 calc R U .
H24B H 0.4554 0.2609 0.2845 0.532 Uiso 1 1 calc R U .
H24C H 0.4247 0.2480 0.3251 0.532 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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 O4 107.8(2) 14 .
O4 Zn1 O2 107.39(14) 14 .
O4 Zn1 O2 107.39(14) . .
O4 Zn1 O1 112.23(12) 14 .
O4 Zn1 O1 112.23(12) . .
O2 Zn1 O1 109.55(17) . .
O4 Zn1 Zn2 125.53(11) 14 .
O4 Zn1 Zn2 76.82(11) . .
O2 Zn1 Zn2 123.21(11) . .
O1 Zn1 Zn2 35.42(5) . .
O4 Zn1 Zn2 76.82(11) 14 14
O4 Zn1 Zn2 125.54(11) . 14
O2 Zn1 Zn2 123.21(11) . 14
O1 Zn1 Zn2 35.42(5) . 14
Zn2 Zn1 Zn2 60.09(3) . 14
O3 Zn2 O5 106.95(14) . .
O3 Zn2 O5 106.95(14) . 16_655
O5 Zn2 O5 109.2(2) . 16_655
O3 Zn2 O1 111.29(19) . .
O5 Zn2 O1 111.16(11) . .
O5 Zn2 O1 111.15(11) 16_655 .
O3 Zn2 Zn1 124.08(13) . .
O5 Zn2 Zn1 75.66(10) . .
O5 Zn2 Zn1 125.28(11) 16_655 .
O1 Zn2 Zn1 35.50(5) . .
O3 Zn2 Zn1 124.08(13) . 3_655
O5 Zn2 Zn1 125.28(11) . 3_655
O5 Zn2 Zn1 75.66(10) 16_655 3_655
O1 Zn2 Zn1 35.50(5) . 3_655
Zn1 Zn2 Zn1 60.85(3) . 3_655
O3 Zn2 Zn2 76.02(16) . 14
O5 Zn2 Zn2 123.81(11) . 14
O5 Zn2 Zn2 123.81(11) 16_655 14
O1 Zn2 Zn2 35.26(9) . 14
Zn1 Zn2 Zn2 59.954(13) . 14
Zn1 Zn2 Zn2 59.954(13) 3_655 14
Zn2 O1 Zn2 109.48(18) . 14
Zn2 O1 Zn1 109.085(15) . .
Zn2 O1 Zn1 109.086(15) 14 .
Zn2 O1 Zn1 109.084(15) . 3_655
Zn2 O1 Zn1 109.085(15) 14 3_655
Zn1 O1 Zn1 111.00(18) . 3_655
C1 O2 Zn1 132.5(5) . .
C9 O5 Zn2 130.6(3) . .
C9 O4 Zn1 130.5(3) . .
C4 O3 Zn2 130.6(5) . .
O2 C1 O2 124.8(8) . 3_655
O2 C1 C2 117.6(4) . .
O2 C1 C2 117.6(4) 3_655 .
C3 C2 C3 118.4(8) 3_655 .
C3 C2 C1 120.8(4) 3_655 .
C3 C2 C1 120.8(4) . .
O4 C9 O5 126.3(4) . .
O4 C9 C10 117.1(5) . .
O5 C9 C10 116.5(5) . .
O3 C4 O3 126.8(9) 14 .
O3 C4 C5 116.6(4) 14 .
O3 C4 C5 116.6(4) . .
C14 C13 C12 122.2(6) . .
C14 C13 C16 106.4(5) . .
C12 C13 C16 131.4(6) . .
C2 C3 C3 120.8(4) . 15_565
C13 C14 C15 119.1(5) . .
C13 C14 C18 115.7(5) . .
C15 C14 C18 125.2(5) . .
C6 C5 C6 118.1(11) . 14
C6 C5 C4 120.9(6) . .
C6 C5 C4 120.9(6) 14 .
C10 C15 C14 117.9(5) . .
C15 C10 C11 121.5(5) . .
C15 C10 C9 118.9(6) . .
C11 C10 C9 119.6(5) . .
C12 C11 C10 120.8(6) . .
C7 C8 C7 113.4(12) 14 .
C7 C8 C8 123.3(6) 14 13_655
C7 C8 C8 123.3(6) . 13_655
C5 C6 C7 118.6(11) . .
C14 C18 C19 108.5(7) . .
C14 C18 C17 99.7(5) . .
C19 C18 C17 112.6(8) . .
C14 C18 C22 109.1(7) . .
C19 C18 C22 114.1(8) . .
C17 C18 C22 111.8(7) . .
C17 C16 C17 120.5(6) 5 .
C17 C16 C13 133.9(5) 5 .
C17 C16 C13 105.6(5) . .
C11 C12 C13 118.4(6) . .
C16 C17 C16 119.5(6) 9 .
C16 C17 C18 128.0(5) 9 .
C16 C17 C18 112.5(5) . .
C8 C7 C6 125.7(12) . .
C18 C22 C23 110.0(9) . .
C20 C19 C18 116.0(10) . .
C19 C20 C21 115.5(14) . .
C24 C23 C22 99.3(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.908(3) 14
Zn1 O4 1.908(3) .
Zn1 O2 1.918(4) .
Zn1 O1 1.936(2) .
Zn1 Zn2 3.1510(8) .
Zn1 Zn2 3.1511(8) 14
Zn2 O3 1.908(5) .
Zn2 O5 1.923(3) .
Zn2 O5 1.923(3) 16_655
Zn2 O1 1.932(2) .
Zn2 Zn1 3.1510(8) 3_655
Zn2 Zn2 3.1555(14) 14
O1 Zn2 1.932(2) 14
O1 Zn1 1.936(2) 3_655
O2 C1 1.242(5) .
O5 C9 1.272(6) .
O4 C9 1.238(6) .
O3 C4 1.249(6) .
C1 O2 1.242(5) 3_655
C1 C2 1.457(11) .
C2 C3 1.379(8) 3_655
C2 C3 1.379(8) .
C9 C10 1.498(7) .
C4 O3 1.249(6) 14
C4 C5 1.491(13) .
C13 C14 1.368(7) .
C13 C12 1.382(8) .
C13 C16 1.548(7) .
C3 C3 1.379(12) 15_565
C14 C15 1.446(7) .
C14 C18 1.483(8) .
C5 C6 1.362(11) .
C5 C6 1.362(11) 14
C15 C10 1.358(7) .
C10 C11 1.396(8) .
C11 C12 1.374(7) .
C8 C7 1.331(12) 14
C8 C7 1.331(12) .
C8 C8 1.42(2) 13_655
C6 C7 1.371(12) .
C18 C19 1.535(12) .
C18 C17 1.544(8) .
C18 C22 1.581(12) .
C16 C17 1.356(7) 5
C16 C17 1.406(7) .
C17 C16 1.356(7) 9
C22 C23 1.684(17) .
C19 C20 1.514(15) .
C20 C21 1.601(13) .
C23 C24 1.558(14) .
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 O2 C1 O2 0.0 . 3_655
Zn1 O2 C1 C2 180.0 . .
O2 C1 C2 C3 180.0 . 3_655
O2 C1 C2 C3 0.0 3_655 3_655
O2 C1 C2 C3 0.0 . .
O2 C1 C2 C3 180.0 3_655 .
Zn1 O4 C9 O5 0.3(9) . .
Zn1 O4 C9 C10 -178.3(4) . .
Zn2 O5 C9 O4 1.8(9) . .
Zn2 O5 C9 C10 -179.6(4) . .
Zn2 O3 C4 O3 0.000(0) . 14
Zn2 O3 C4 C5 180.000(0) . .
C3 C2 C3 C3 0.0 3_655 15_565
C1 C2 C3 C3 180.0 . 15_565
C12 C13 C14 C15 0.2(14) . .
C16 C13 C14 C15 -178.6(7) . .
C12 C13 C14 C18 -178.4(9) . .
C16 C13 C14 C18 2.8(11) . .
O3 C4 C5 C6 180.000(0) 14 .
O3 C4 C5 C6 0.000(1) . .
O3 C4 C5 C6 0.000(0) 14 14
O3 C4 C5 C6 180.000(0) . 14
C13 C14 C15 C10 -0.8(12) . .
C18 C14 C15 C10 177.6(8) . .
C14 C15 C10 C11 0.5(12) . .
C14 C15 C10 C9 -179.4(6) . .
O4 C9 C10 C15 172.4(7) . .
O5 C9 C10 C15 -6.3(9) . .
O4 C9 C10 C11 -7.6(10) . .
O5 C9 C10 C11 173.7(7) . .
C15 C10 C11 C12 0.4(14) . .
C9 C10 C11 C12 -179.6(8) . .
C6 C5 C6 C7 0.000(1) 14 .
C4 C5 C6 C7 180.000(0) . .
C13 C14 C18 C19 116.2(9) . .
C15 C14 C18 C19 -62.3(11) . .
C13 C14 C18 C17 -1.8(11) . .
C15 C14 C18 C17 179.8(8) . .
C13 C14 C18 C22 -119.0(9) . .
C15 C14 C18 C22 62.6(11) . .
C14 C13 C16 C17 178.3(10) . 5
C12 C13 C16 C17 -0.3(19) . 5
C14 C13 C16 C17 -2.6(10) . .
C12 C13 C16 C17 178.7(10) . .
C10 C11 C12 C13 -1.1(15) . .
C14 C13 C12 C11 0.8(16) . .
C16 C13 C12 C11 179.2(9) . .
C17 C16 C17 C16 -0.8(19) 5 9
C13 C16 C17 C16 180.0(7) . 9
C17 C16 C17 C18 -179.2(7) 5 .
C13 C16 C17 C18 1.7(10) . .
C14 C18 C17 C16 -178.3(9) . 9
C19 C18 C17 C16 66.8(12) . 9
C22 C18 C17 C16 -63.1(12) . 9
C14 C18 C17 C16 -0.1(10) . .
C19 C18 C17 C16 -115.0(8) . .
C22 C18 C17 C16 115.0(8) . .
C7 C8 C7 C6 0.000(0) 14 .
C8 C8 C7 C6 180.000(0) 13_655 .
C5 C6 C7 C8 0.000(1) . .
C14 C18 C22 C23 56.9(9) . .
C19 C18 C22 C23 178.5(8) . .
C17 C18 C22 C23 -52.3(10) . .
C14 C18 C19 C20 -56.4(11) . .
C17 C18 C19 C20 53.0(11) . .
C22 C18 C19 C20 -178.2(9) . .
C18 C19 C20 C21 174.7(10) . .
C18 C22 C23 C24 179.0(9) . .
