#------------------------------------------------------------------------------
#$Date: 2019-11-25 04:51:04 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240048 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/93/4129300.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_4129300
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            'C83 H90 O13 Zn4'
_chemical_formula_weight         1557.02
_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                   29.9363(5)
_cell_length_b                   29.9363(5)
_cell_length_c                   29.9363(5)
_cell_measurement_reflns_used    84796
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.01
_cell_measurement_theta_min      6.62
_cell_volume                     26828.4(8)
_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 0.994
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            135481
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.063
_diffrn_reflns_theta_min         6.613
_diffrn_source                   'Rigaku MM007 rotating anode'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.750040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    0.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4872
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.652
_exptl_crystal_size_min          0.586
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.038
_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     231
_refine_ls_number_reflns         9304
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0594P)²+6.7233P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8801
_reflns_number_total             9304
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b00365_si_002.cif
_cod_data_source_block           MUF-77-Butyl
_cod_original_cell_volume        26828.4(13)
_cod_database_code               4129300
_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   0.598
_shelx_estimated_absorpt_t_max   0.645
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'x, y, -z'
'-x, y, z'
'x, -y, 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_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 0.32269(2) 0.0000 0.44665(2) 0.03538(9) Uani 1 2 d S T P . .
Zn2 Zn 0.24861(2) 0.05319(2) 0.5000 0.03703(9) Uani 1 2 d S T P . .
O1 O 0.28565(5) 0.0000 0.5000 0.0318(3) Uani 1 4 d S T P . .
O5 O 0.25907(5) 0.08899(4) 0.44723(4) 0.0691(4) Uani 1 1 d . . . . .
O4 O 0.31223(4) 0.05238(4) 0.41069(4) 0.0681(3) Uani 1 1 d . . . . .
C1 C 0.40390(9) 0.0000 0.5000 0.0528(7) Uani 1 4 d S T P . .
O2 O 0.38504(5) 0.0000 0.46296(6) 0.0671(5) Uani 1 2 d S T P . .
O3 O 0.18637(5) 0.03712(7) 0.5000 0.0827(6) Uani 1 2 d S T P . .
C4 C 0.16771(10) 0.0000 0.5000 0.0676(10) Uani 1 4 d S T P . .
C9 C 0.28578(6) 0.08393(6) 0.41535(6) 0.0596(4) Uani 1 1 d . . . . .
C2 C 0.45394(10) 0.0000 0.5000 0.0597(9) Uani 1 4 d S T P . .
C3 C 0.47672(8) 0.0000 0.46039(10) 0.0877(10) Uani 1 2 d S T P . .
H3 H 0.4612 0.0000 0.4335 0.105 Uiso 1 2 calc R U P . .
C13 C 0.28611(8) 0.18371(8) 0.31286(8) 0.0899(8) Uani 1 1 d . . . . .
C14 C 0.25388(7) 0.18434(8) 0.34606(7) 0.0830(7) Uani 1 1 d . . . . .
C15 C 0.25382(7) 0.15209(7) 0.37965(7) 0.0816(7) Uani 1 1 d . . . . .
H15 H 0.2323 0.1530 0.4021 0.098 Uiso 1 1 calc R U . . .
C10 C 0.28557(7) 0.11897(7) 0.37953(7) 0.0754(6) Uani 1 1 d . . . . .
C11 C 0.31764(9) 0.11826(8) 0.34609(8) 0.1018(9) Uani 1 1 d . . . . .
H11 H 0.3391 0.0958 0.3459 0.122 Uiso 1 1 calc R U . . .
C16 C 0.27714(8) 0.22247(8) 0.28233(8) 0.0873(8) Uani 1 1 d . . . . .
C18 C 0.22095(8) 0.22176(8) 0.34087(8) 0.0940(8) Uani 1 1 d . . . . .
C17 C 0.23880(8) 0.24436(8) 0.29870(8) 0.0868(7) Uani 1 1 d . . . . .
C12 C 0.31812(9) 0.15053(9) 0.31305(9) 0.1170(12) Uani 1 1 d . . . . .
H12 H 0.3400 0.1499 0.2910 0.140 Uiso 1 1 calc R U . . .
C5 C 0.11791(11) 0.0000 0.5000 0.0942(16) Uani 1 4 d S T P . .
C19 C 0.22253(13) 0.25167(11) 0.38219(10) 0.1238(13) Uani 1 1 d . . . . .
H19A H 0.2006 0.2753 0.3789 0.149 Uiso 1 1 calc R U . . .
H19B H 0.2144 0.2341 0.4082 0.149 Uiso 1 1 calc R U . . .
C24 C 0.16946(17) 0.1718(2) 0.2939(2) 0.199(2) Uani 1 1 d D . . . .
H24A H 0.1912 0.1478 0.2954 0.239 Uiso 1 1 calc R U . . .
H24B H 0.1751 0.1889 0.2670 0.239 Uiso 1 1 calc R U . . .
C23 C 0.17411(10) 0.20165(12) 0.33468(14) 0.1283(14) Uani 1 1 d . . . . .
H23A H 0.1666 0.1844 0.3611 0.154 Uiso 1 1 calc R U . . .
H23B H 0.1527 0.2258 0.3323 0.154 Uiso 1 1 calc R U . . .
C6 C 0.09478(11) 0.03831(15) 0.5000 0.182(3) Uani 1 2 d S T P . .
H6 H 0.1100 0.0654 0.5000 0.218 Uiso 1 2 calc R U P . .
C20 C 0.2676(2) 0.27237(17) 0.39000(17) 0.191(2) Uani 1 1 d D . . . .
H20A H 0.2774 0.2872 0.3629 0.229 Uiso 1 1 calc R U . . .
H20B H 0.2890 0.2490 0.3969 0.229 Uiso 1 1 calc R U . . .
C8 C 0.02487(12) 0.0000 0.5000 0.138(3) Uani 1 4 d S T P . .
C7 C 0.04811(11) 0.03814(16) 0.5000 0.202(4) Uani 1 2 d S T P . .
H7 H 0.0329 0.0652 0.5000 0.242 Uiso 1 2 calc R U P . .
C21 C 0.2668(4) 0.3077(4) 0.4299(4) 0.364(5) Uiso 1 1 d D . . . .
H21A H 0.2447 0.3307 0.4245 0.437 Uiso 1 1 calc R U . . .
H21B H 0.2604 0.2932 0.4581 0.437 Uiso 1 1 calc R U . . .
C22 C 0.3157(6) 0.3278(5) 0.4295(6) 0.658(13) Uiso 1 1 d D . . . .
H22A H 0.3185 0.3495 0.4530 0.987 Uiso 1 1 calc R U . . .
H22B H 0.3213 0.3418 0.4013 0.987 Uiso 1 1 calc R U . . .
H22C H 0.3369 0.3042 0.4342 0.987 Uiso 1 1 calc R U . . .
C25 C 0.1198(4) 0.1513(4) 0.2924(4) 0.378(6) Uiso 1 1 d D . . . .
H25A H 0.1143 0.1293 0.3155 0.453 Uiso 0.632(10) 1 calc R U P A 1
H25B H 0.0966 0.1740 0.2926 0.453 Uiso 0.632(10) 1 calc R U P A 1
H25C H 0.1058 0.1489 0.3215 0.453 Uiso 0.368(10) 1 calc R U P A 2
H25D H 0.1177 0.1234 0.2762 0.453 Uiso 0.368(10) 1 calc R U P A 2
C26A C 0.1278(7) 0.1297(7) 0.2441(7) 0.500(13) Uiso 0.632(10) 1 d D . P A 1
H26A H 0.1339 0.1530 0.2229 0.750 Uiso 0.632(10) 1 calc R U P A 1
H26B H 0.1015 0.1137 0.2350 0.750 Uiso 0.632(10) 1 calc R U P A 1
H26C H 0.1527 0.1096 0.2454 0.750 Uiso 0.632(10) 1 calc R U P A 1
C26B C 0.1031(9) 0.1952(10) 0.2634(12) 0.500(13) Uiso 0.368(10) 1 d D . P A 2
H26D H 0.1080 0.2218 0.2805 0.750 Uiso 0.368(10) 1 calc R U P A 2
H26E H 0.0718 0.1924 0.2568 0.750 Uiso 0.368(10) 1 calc R U P A 2
H26F H 0.1197 0.1968 0.2360 0.750 Uiso 0.368(10) 1 calc R U P A 2
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 108.88(9) . 24
O4 Zn1 O2 107.36(5) . .
O4 Zn1 O2 107.36(5) 24 .
O4 Zn1 O1 111.48(4) . .
O4 Zn1 O1 111.48(4) 24 .
O2 Zn1 O1 110.11(6) . .
O3 Zn2 O5 107.17(5) . .
O3 Zn2 O5 107.17(5) . 22_556
O5 Zn2 O5 109.49(9) . 22_556
O3 Zn2 O1 110.38(7) . .
O5 Zn2 O1 111.24(4) . .
O5 Zn2 O1 111.23(4) 22_556 .
Zn2 O1 Zn2 110.29(8) . 11_556
Zn2 O1 Zn1 109.020(5) . .
Zn2 O1 Zn1 109.019(5) 11_556 .
Zn2 O1 Zn1 109.021(5) . 22_556
Zn2 O1 Zn1 109.020(5) 11_556 22_556
Zn1 O1 Zn1 110.46(8) . 22_556
C9 O5 Zn2 131.11(11) . .
C9 O4 Zn1 131.32(11) . .
O2 C1 O2 126.0(3) . 22_556
O2 C1 C2 116.99(13) . .
O2 C1 C2 116.99(13) 22_556 .
C1 O2 Zn1 131.66(16) . .
C4 O3 Zn2 131.17(18) . .
O3 C4 O3 126.6(3) 11_556 .
O3 C4 C5 116.70(15) 11_556 .
O3 C4 C5 116.69(15) . .
O4 C9 O5 125.78(15) . .
O4 C9 C10 117.04(15) . .
O5 C9 C10 117.18(15) . .
C3 C2 C3 120.2(3) . 22_556
C3 C2 C1 119.90(15) . .
C3 C2 C1 119.90(15) 22_556 .
C2 C3 C3 119.90(15) . 10_655
C12 C13 C14 119.37(18) . .
C12 C13 C16 133.07(18) . .
C14 C13 C16 107.57(16) . .
C13 C14 C15 120.61(17) . .
C13 C14 C18 113.17(16) . .
C15 C14 C18 126.22(17) . .
C10 C15 C14 119.81(17) . .
C15 C10 C11 119.46(17) . .
C15 C10 C9 120.39(17) . .
C11 C10 C9 120.15(16) . .
C12 C11 C10 120.84(18) . .
C17 C16 C17 119.80(18) 2 .
C17 C16 C13 133.15(17) 2 .
C17 C16 C13 107.05(16) . .
C14 C18 C19 109.5(2) . .
C14 C18 C17 100.74(15) . .
C19 C18 C17 113.5(2) . .
C14 C18 C23 108.6(2) . .
C19 C18 C23 110.8(2) . .
C17 C18 C23 113.1(2) . .
C16 C17 C16 120.19(18) 3 .
C16 C17 C18 128.32(17) 3 .
C16 C17 C18 111.47(16) . .
C13 C12 C11 119.90(19) . .
C6 C5 C6 117.8(4) 11_556 .
C6 C5 C4 121.1(2) 11_556 .
C6 C5 C4 121.1(2) . .
C20 C19 C18 113.3(3) . .
C23 C24 C25 109.4(6) . .
C24 C23 C18 114.3(3) . .
C5 C6 C7 120.9(4) . .
C19 C20 C21 112.1(6) . .
C7 C8 C7 117.3(4) . 11_556
C7 C8 C8 121.4(2) . 13_556
C7 C8 C8 121.4(2) 11_556 13_556
C8 C7 C6 121.6(4) . .
C22 C21 C20 103.5(9) . .
C26A C25 C24 92.3(11) . .
C24 C25 C26B 89.5(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.9276(11) .
Zn1 O4 1.9277(11) 24
Zn1 O2 1.9292(14) .
Zn1 O1 1.9443(9) .
Zn2 O3 1.9243(16) .
Zn2 O5 1.9345(11) .
Zn2 O5 1.9346(11) 22_556
Zn2 O1 1.9403(9) .
O1 Zn2 1.9403(9) 11_556
O1 Zn1 1.9444(9) 22_556
O5 C9 1.254(2) .
O4 C9 1.240(2) .
C1 O2 1.244(2) .
C1 O2 1.244(2) 22_556
C1 C2 1.498(4) .
O3 C4 1.244(2) .
C4 O3 1.244(2) 11_556
C4 C5 1.491(4) .
C9 C10 1.500(2) .
C2 C3 1.368(3) .
C2 C3 1.368(3) 22_556
C3 C3 1.394(5) 10_655
C13 C12 1.380(3) .
C13 C14 1.385(3) .
C13 C16 1.501(2) .
C14 C15 1.394(3) .
C14 C18 1.500(3) .
C15 C10 1.374(3) .
C10 C11 1.387(3) .
C11 C12 1.383(3) .
C16 C17 1.395(3) 2
C16 C17 1.410(3) .
C18 C19 1.528(4) .
C18 C17 1.529(2) .
C18 C23 1.537(4) .
C17 C16 1.395(3) 3
C5 C6 1.339(4) 11_556
C5 C6 1.340(4) .
C19 C20 1.503(6) .
C24 C23 1.519(6) .
C24 C25 1.610(11) .
C6 C7 1.397(4) .
C20 C21 1.594(10) .
C8 C7 1.337(5) .
C8 C7 1.337(5) 11_556
C8 C8 1.489(7) 13_556
C21 C22 1.581(13) .
C25 C26A 1.603(18) .
C25 C26B 1.65(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
O2 C1 O2 Zn1 0.000(0) 22_556 .
C2 C1 O2 Zn1 180.000(0) . .
Zn2 O3 C4 O3 0.0 . 11_556
Zn2 O3 C4 C5 180.0 . .
Zn1 O4 C9 O5 1.6(3) . .
Zn1 O4 C9 C10 -178.04(15) . .
Zn2 O5 C9 O4 1.2(3) . .
Zn2 O5 C9 C10 -179.20(15) . .
O2 C1 C2 C3 0.000(0) . .
O2 C1 C2 C3 180.000(0) 22_556 .
O2 C1 C2 C3 180.000(0) . 22_556
O2 C1 C2 C3 0.000(0) 22_556 22_556
C3 C2 C3 C3 0.000(0) 22_556 10_655
C1 C2 C3 C3 180.000(0) . 10_655
C12 C13 C14 C15 0.5(5) . .
C16 C13 C14 C15 -179.8(3) . .
C12 C13 C14 C18 -178.9(3) . .
C16 C13 C14 C18 0.8(4) . .
C13 C14 C15 C10 -1.0(4) . .
C18 C14 C15 C10 178.3(3) . .
C14 C15 C10 C11 0.6(4) . .
C14 C15 C10 C9 -179.7(2) . .
O4 C9 C10 C15 172.5(2) . .
O5 C9 C10 C15 -7.2(3) . .
O4 C9 C10 C11 -7.8(3) . .
O5 C9 C10 C11 172.6(2) . .
C15 C10 C11 C12 0.2(5) . .
C9 C10 C11 C12 -179.5(3) . .
C12 C13 C16 C17 -1.8(6) . 2
C14 C13 C16 C17 178.6(3) . 2
C12 C13 C16 C17 178.7(4) . .
C14 C13 C16 C17 -0.9(3) . .
C13 C14 C18 C19 -120.2(3) . .
C15 C14 C18 C19 60.4(4) . .
C13 C14 C18 C17 -0.4(3) . .
C15 C14 C18 C17 -179.8(3) . .
C13 C14 C18 C23 118.7(3) . .
C15 C14 C18 C23 -60.7(4) . .
C17 C16 C17 C16 -0.2(6) 2 3
C13 C16 C17 C16 179.4(2) . 3
C17 C16 C17 C18 -178.9(2) 2 .
C13 C16 C17 C18 0.7(3) . .
C14 C18 C17 C16 -178.8(3) . 3
C19 C18 C17 C16 -61.9(4) . 3
C23 C18 C17 C16 65.4(4) . 3
C14 C18 C17 C16 -0.2(3) . .
C19 C18 C17 C16 116.7(3) . .
C23 C18 C17 C16 -116.0(3) . .
C14 C13 C12 C11 0.3(5) . .
C16 C13 C12 C11 -179.3(3) . .
C10 C11 C12 C13 -0.7(5) . .
O3 C4 C5 C6 0.0 11_556 11_556
O3 C4 C5 C6 180.0 . 11_556
O3 C4 C5 C6 180.0 11_556 .
O3 C4 C5 C6 0.0 . .
C14 C18 C19 C20 60.2(3) . .
C17 C18 C19 C20 -51.4(3) . .
C23 C18 C19 C20 -180.0(3) . .
C25 C24 C23 C18 177.6(6) . .
C14 C18 C23 C24 -60.3(3) . .
C19 C18 C23 C24 179.4(3) . .
C17 C18 C23 C24 50.6(4) . .
C6 C5 C6 C7 0.0 11_556 .
C4 C5 C6 C7 180.0 . .
C18 C19 C20 C21 173.4(5) . .
C7 C8 C7 C6 0.0 11_556 .
C8 C8 C7 C6 180.0 13_556 .
C5 C6 C7 C8 0.0 . .
C19 C20 C21 C22 -175.5(9) . .
C23 C24 C25 C26A 172.8(10) . .
C23 C24 C25 C26B 89.1(15) . .
