#------------------------------------------------------------------------------
#$Date: 2019-11-25 04:51:04 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240048 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/93/4129303.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_4129303
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            'C131 H186 O13 Zn4'
_chemical_formula_weight         2230.27
_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                   29.8062(3)
_cell_length_b                   29.8062(3)
_cell_length_c                   29.8062(3)
_cell_measurement_reflns_used    49874
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.13
_cell_measurement_theta_min      6.64
_cell_volume                     26480.1(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.989
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59507
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.118
_diffrn_reflns_theta_min         6.642
_diffrn_source                   'Rigaku MM007 rotating anode'
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.700167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.839
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7176
_exptl_crystal_size_max          0.488
_exptl_crystal_size_mid          0.433
_exptl_crystal_size_min          0.415
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         9137
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.1115
_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)+(0.1837P)²+43.9337P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3743
_refine_ls_wR_factor_ref         0.3777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7900
_reflns_number_total             9137
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b00365_si_002.cif
_cod_data_source_block           MUF-77-Decyl
_cod_original_cell_volume        26480.1(8)
_cod_database_code               4129303
_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   0.660
_shelx_estimated_absorpt_t_max   0.699
_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 0.0000 0.32278(3) 0.44645(3) 0.0669(3) Uani 1 2 d S T P
Zn2 Zn 0.05300(3) 0.24849(3) 0.5000 0.0702(4) Uani 1 2 d S T P
O1 O 0.0000 0.2860(2) 0.5000 0.0618(15) Uani 1 4 d S T P
O2 O 0.0000 0.38514(19) 0.4628(2) 0.109(2) Uani 1 2 d S T P
O3 O 0.05160(17) 0.31183(18) 0.40976(17) 0.1087(16) Uani 1 1 d . . .
C1 C 0.0000 0.4042(4) 0.5000 0.091(4) Uani 1 4 d S T P
O5 O 0.08766(17) 0.25881(19) 0.44660(18) 0.1103(16) Uani 1 1 d . . .
O6 O 0.0374(3) 0.1856(2) 0.5000 0.126(3) Uani 1 2 d S T P
C4 C 0.0000 0.1667(4) 0.5000 0.105(4) Uani 1 4 d S T P
C9 C 0.0827(3) 0.2855(3) 0.4153(3) 0.101(2) Uani 1 1 d . . .
C2 C 0.0000 0.4530(4) 0.5000 0.097(4) Uani 1 4 d S T P
C13 C 0.1802(4) 0.2834(3) 0.3110(4) 0.158(5) Uani 1 1 d . . .
C11 C 0.1161(4) 0.3156(4) 0.3437(4) 0.169(5) Uani 1 1 d . . .
H11 H 0.0933 0.3369 0.3434 0.202 Uiso 1 1 calc R U .
C14 C 0.1828(4) 0.2509(3) 0.3430(4) 0.150(4) Uani 1 1 d . . .
C15 C 0.1496(3) 0.2521(3) 0.3783(3) 0.135(3) Uani 1 1 d . . .
H15 H 0.1504 0.2311 0.4013 0.162 Uiso 1 1 calc R U .
C10 C 0.1173(3) 0.2843(3) 0.3776(3) 0.130(3) Uani 1 1 d . . .
C5 C 0.0000 0.1183(5) 0.5000 0.145(8) Uani 1 4 d S T P
C0AA C 0.0000 0.4771(3) 0.4599(4) 0.138(5) Uani 1 2 d S T P
H0AA H 0.0000 0.4617 0.4328 0.166 Uiso 1 2 calc R U P
C18 C 0.2186(4) 0.2182(4) 0.3383(4) 0.170(5) Uani 1 1 d . . .
C16 C 0.2193(3) 0.2745(4) 0.2787(4) 0.158(5) Uani 1 1 d . . .
C17 C 0.2413(4) 0.2361(4) 0.2956(3) 0.149(4) Uani 1 1 d . . .
C12 C 0.1475(4) 0.3162(4) 0.3106(5) 0.219(8) Uani 1 1 d . . .
H12 H 0.1469 0.3380 0.2883 0.263 Uiso 1 1 calc R U .
C8 C 0.0000 0.0242(6) 0.5000 0.233(18) Uani 1 4 d S T P
C7 C 0.0367(7) 0.0475(5) 0.5000 0.222(11) Uani 1 2 d S T P
H7 H 0.0635 0.0315 0.5000 0.266 Uiso 1 2 calc R U P
C6 C 0.0401(7) 0.0958(4) 0.5000 0.223(11) Uani 1 2 d S T P
H6 H 0.0676 0.1107 0.5000 0.267 Uiso 1 2 calc R U P
C22 C 0.1992(6) 0.1708(4) 0.3325(6) 0.214(8) Uani 1 1 d . . .
H22A H 0.1857 0.1614 0.3605 0.257 Uiso 1 1 calc R U .
H22B H 0.2236 0.1502 0.3258 0.257 Uiso 1 1 calc R U .
C19 C 0.2505(5) 0.2205(6) 0.3789(4) 0.211(8) Uani 1 1 d . . .
H19A H 0.2746 0.1991 0.3743 0.253 Uiso 1 1 calc R U .
H19B H 0.2341 0.2113 0.4054 0.253 Uiso 1 1 calc R U .
C20 C 0.2722(12) 0.2689(12) 0.3881(13) 0.397(14) Uiso 1 1 d D . .
H20A H 0.2860 0.2791 0.3604 0.476 Uiso 1 1 calc R U .
H20B H 0.2479 0.2896 0.3948 0.476 Uiso 1 1 calc R U .
C21 C 0.3079(15) 0.2729(16) 0.4265(16) 0.58(3) Uiso 1 1 d D . .
H21A H 0.3186 0.3033 0.4281 0.870 Uiso 1 1 calc R U .
H21B H 0.3326 0.2532 0.4203 0.870 Uiso 1 1 calc R U .
H21C H 0.2945 0.2648 0.4546 0.870 Uiso 1 1 calc R U .
C23 C 0.1634(12) 0.1672(12) 0.2945(12) 0.397(14) Uiso 1 1 d D . .
H23A H 0.1744 0.1836 0.2687 0.476 Uiso 1 1 calc R U .
H23B H 0.1365 0.1824 0.3048 0.476 Uiso 1 1 calc R U .
C24 C 0.1493(15) 0.1183(14) 0.2779(14) 0.56(3) Uiso 1 1 d D . .
H24A H 0.1270 0.1208 0.2548 0.835 Uiso 1 1 calc R U .
H24B H 0.1372 0.1016 0.3027 0.835 Uiso 1 1 calc R U .
H24C H 0.1752 0.1031 0.2663 0.835 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
O3 Zn1 O3 106.8(4) 16 .
O3 Zn1 O2 108.1(2) 16 .
O3 Zn1 O2 108.1(2) . .
O3 Zn1 O1 111.97(17) 16 .
O3 Zn1 O1 111.97(17) . .
O2 Zn1 O1 109.8(3) . .
O3 Zn1 Zn2 124.86(16) 16 .
O3 Zn1 Zn2 76.54(15) . .
O2 Zn1 Zn2 123.40(17) . .
O1 Zn1 Zn2 35.43(8) . .
O3 Zn1 Zn2 76.53(15) 16 3_556
O3 Zn1 Zn2 124.86(16) . 3_556
O2 Zn1 Zn2 123.40(17) . 3_556
O1 Zn1 Zn2 35.43(8) . 3_556
Zn2 Zn1 Zn2 60.12(4) . 3_556
O5 Zn2 O5 111.8(4) 14_556 .
O5 Zn2 O6 106.6(2) 14_556 .
O5 Zn2 O6 106.6(2) . .
O5 Zn2 O1 110.27(16) 14_556 .
O5 Zn2 O1 110.27(16) . .
O6 Zn2 O1 111.3(3) . .
O5 Zn2 Zn1 74.80(15) 14_556 14_556
O5 Zn2 Zn1 125.16(16) . 14_556
O6 Zn2 Zn1 124.1(2) . 14_556
O1 Zn2 Zn1 35.48(7) . 14_556
O5 Zn2 Zn1 125.16(16) 14_556 .
O5 Zn2 Zn1 74.80(15) . .
O6 Zn2 Zn1 124.1(2) . .
O1 Zn2 Zn1 35.48(7) . .
Zn1 Zn2 Zn1 60.81(4) 14_556 .
O5 Zn2 Zn2 122.51(17) 14_556 3_556
O5 Zn2 Zn2 122.51(17) . 3_556
O6 Zn2 Zn2 76.0(3) . 3_556
O1 Zn2 Zn2 35.26(15) . 3_556
Zn1 Zn2 Zn2 59.939(19) 14_556 3_556
Zn1 Zn2 Zn2 59.940(19) . 3_556
Zn2 O1 Zn2 109.5(3) . 3_556
Zn2 O1 Zn1 109.09(2) . 14_556
Zn2 O1 Zn1 109.09(2) 3_556 14_556
Zn2 O1 Zn1 109.09(2) . .
Zn2 O1 Zn1 109.09(2) 3_556 .
Zn1 O1 Zn1 111.0(3) 14_556 .
C1 O2 Zn1 131.9(7) . .
C9 O3 Zn1 129.8(5) . .
O2 C1 O2 125.6(11) . 14_556
O2 C1 C2 117.2(6) . .
O2 C1 C2 117.2(6) 14_556 .
C9 O5 Zn2 131.7(5) . .
C4 O6 Zn2 130.8(8) . .
O6 C4 O6 126.4(12) . 3_556
O6 C4 C5 116.8(6) . .
O6 C4 C5 116.8(6) 3_556 .
O3 C9 O5 127.2(6) . .
O3 C9 C10 115.3(7) . .
O5 C9 C10 117.4(7) . .
C0AA C2 C0AA 118.0(12) . 14_556
C0AA C2 C1 121.0(6) . .
C0AA C2 C1 121.0(6) 14_556 .
C14 C13 C12 123.4(9) . .
C14 C13 C16 105.7(7) . .
C12 C13 C16 130.9(8) . .
C12 C11 C10 121.6(8) . .
C13 C14 C15 116.9(8) . .
C13 C14 C18 116.9(8) . .
C15 C14 C18 126.2(7) . .
C10 C15 C14 119.5(8) . .
C15 C10 C11 120.5(7) . .
C15 C10 C9 119.0(8) . .
C11 C10 C9 120.5(7) . .
C6 C5 C6 121.6(17) 3_556 .
C6 C5 C4 119.2(8) 3_556 .
C6 C5 C4 119.2(8) . .
C0AA C0AA C2 121.0(6) 2_565 .
C14 C18 C22 110.6(11) . .
C14 C18 C17 99.8(7) . .
C22 C18 C17 113.0(12) . .
C14 C18 C19 110.5(12) . .
C22 C18 C19 111.3(11) . .
C17 C18 C19 111.3(11) . .
C17 C16 C17 119.4(8) 9 .
C17 C16 C13 134.8(8) 9 .
C17 C16 C13 105.8(7) . .
C16 C17 C16 120.6(8) 5 .
C16 C17 C18 127.6(8) 5 .
C16 C17 C18 111.8(7) . .
C11 C12 C13 118.0(9) . .
C7 C8 C7 115.3(19) 3_556 .
C7 C8 C8 122.3(10) 3_556 13_556
C7 C8 C8 122.3(10) . 13_556
C8 C7 C6 126.3(18) . .
C5 C6 C7 115.2(17) . .
C18 C22 C23 113.8(17) . .
C18 C19 C20 115.0(17) . .
C21 C20 C19 118(3) . .
C22 C23 C24 118(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O3 1.915(4) 16
Zn1 O3 1.915(4) .
Zn1 O2 1.922(6) .
Zn1 O1 1.937(4) .
Zn1 Zn2 3.1537(11) .
Zn1 Zn2 3.1537(11) 3_556
Zn2 O5 1.922(5) 14_556
Zn2 O5 1.922(5) .
Zn2 O6 1.932(7) .
Zn2 O1 1.935(4) .
Zn2 Zn1 3.1536(11) 14_556
Zn2 Zn2 3.159(2) 3_556
O1 Zn2 1.935(4) 3_556
O1 Zn1 1.937(4) 14_556
O2 C1 1.245(8) .
O3 C9 1.226(8) .
C1 O2 1.245(8) 14_556
C1 C2 1.455(16) .
O5 C9 1.235(9) .
O6 C4 1.247(9) .
C4 O6 1.247(9) 3_556
C4 C5 1.445(18) .
C9 C10 1.525(10) .
C2 C0AA 1.394(13) .
C2 C0AA 1.394(13) 14_556
C13 C14 1.363(11) .
C13 C12 1.380(12) .
C13 C16 1.534(11) .
C11 C12 1.361(12) .
C11 C10 1.377(12) .
C14 C15 1.445(11) .
C14 C18 1.452(12) .
C15 C10 1.358(11) .
C5 C6 1.370(18) 3_556
C5 C6 1.370(18) .
C0AA C0AA 1.364(19) 2_565
C18 C22 1.54(2) .
C18 C17 1.538(11) .
C18 C19 1.54(2) .
C16 C17 1.375(11) 9
C16 C17 1.412(11) .
C17 C16 1.375(11) 5
C8 C7 1.30(2) 3_556
C8 C7 1.30(2) .
C8 C8 1.44(4) 13_556
C7 C6 1.445(18) .
C22 C23 1.56(3) .
C19 C20 1.61(3) .
C20 C21 1.568(19) .
C23 C24 1.594(19) .
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 0.000(3) . 14_556
Zn1 O2 C1 C2 180.000(2) . .
Zn2 O6 C4 O6 0.0 . 3_556
Zn2 O6 C4 C5 180.0 . .
Zn1 O3 C9 O5 0.8(13) . .
Zn1 O3 C9 C10 177.2(6) . .
Zn2 O5 C9 O3 -3.5(14) . .
Zn2 O5 C9 C10 -179.8(6) . .
O2 C1 C2 C0AA 0.000(3) . .
O2 C1 C2 C0AA 180.000(3) 14_556 .
O2 C1 C2 C0AA 180.000(3) . 14_556
O2 C1 C2 C0AA 0.000(4) 14_556 14_556
C12 C13 C14 C15 -1(2) . .
C16 C13 C14 C15 179.1(11) . .
C12 C13 C14 C18 178.8(15) . .
C16 C13 C14 C18 -0.9(18) . .
C13 C14 C15 C10 1.6(19) . .
C18 C14 C15 C10 -178.4(13) . .
C14 C15 C10 C11 -0.3(19) . .
C14 C15 C10 C9 -179.6(10) . .
C12 C11 C10 C15 -2(2) . .
C12 C11 C10 C9 177.7(14) . .
O3 C9 C10 C15 -171.7(10) . .
O5 C9 C10 C15 5.0(14) . .
O3 C9 C10 C11 9.0(15) . .
O5 C9 C10 C11 -174.2(11) . .
O6 C4 C5 C6 180.0 . 3_556
O6 C4 C5 C6 0.0 3_556 3_556
O6 C4 C5 C6 0.0 . .
O6 C4 C5 C6 180.0 3_556 .
C0AA C2 C0AA C0AA 0.000(6) 14_556 2_565
C1 C2 C0AA C0AA 180.000(3) . 2_565
C13 C14 C18 C22 -118.2(14) . .
C15 C14 C18 C22 61.8(19) . .
C13 C14 C18 C17 1.0(17) . .
C15 C14 C18 C17 -179.0(13) . .
C13 C14 C18 C19 118.2(14) . .
C15 C14 C18 C19 -61.9(18) . .
C14 C13 C16 C17 -177.0(16) . 9
C12 C13 C16 C17 3(3) . 9
C14 C13 C16 C17 0.4(16) . .
C12 C13 C16 C17 -179.3(16) . .
C17 C16 C17 C16 -1(3) 9 5
C13 C16 C17 C16 -179.1(11) . 5
C17 C16 C17 C18 178.0(11) 9 .
C13 C16 C17 C18 0.2(16) . .
C14 C18 C17 C16 178.6(15) . 5
C22 C18 C17 C16 -64.0(19) . 5
C19 C18 C17 C16 62.0(19) . 5
C14 C18 C17 C16 -0.7(16) . .
C22 C18 C17 C16 116.7(13) . .
C19 C18 C17 C16 -117.2(13) . .
C10 C11 C12 C13 2(3) . .
C14 C13 C12 C11 -1(3) . .
C16 C13 C12 C11 179.1(15) . .
C7 C8 C7 C6 0.0 3_556 .
C8 C8 C7 C6 180.0 13_556 .
C6 C5 C6 C7 0.0 3_556 .
C4 C5 C6 C7 180.0 . .
C8 C7 C6 C5 0.0 . .
C14 C18 C22 C23 51.7(19) . .
C17 C18 C22 C23 -59.1(19) . .
C19 C18 C22 C23 174.9(16) . .
C14 C18 C19 C20 -56.2(18) . .
C22 C18 C19 C20 -179.4(16) . .
C17 C18 C19 C20 53.6(19) . .
C18 C19 C20 C21 -175(3) . .
C18 C22 C23 C24 166(3) . .
