#------------------------------------------------------------------------------
#$Date: 2019-11-25 04:51:04 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240048 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/92/4129299.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_4129299
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            'C67 H58 O13 Zn4'
_chemical_formula_weight         1332.61
_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                   29.9508(5)
_cell_length_b                   29.9508(5)
_cell_length_c                   29.9508(5)
_cell_measurement_reflns_used    93755
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      57.05
_cell_measurement_theta_min      6.61
_cell_volume                     26867.4(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 0.993
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            135510
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.042
_diffrn_reflns_theta_min         6.610
_diffrn_source                   'Rigaku MM007 rotating anode'
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.741995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    0.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.252
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.033
_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     213
_refine_ls_number_reflns         9309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0418P)²+10.5494P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8194
_reflns_number_total             9309
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b00365_si_002.cif
_cod_data_source_block           MUF-77-Ethyl
_cod_original_cell_volume        26867.4(13)
_cod_database_code               4129299
_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   0.809
_shelx_estimated_absorpt_t_max   0.827
_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 0.32269(2) 0.44658(2) 0.0000 0.03660(9) Uani 1 2 d S T P
Zn2 Zn 0.24861(2) 0.5000 0.05306(2) 0.03846(9) Uani 1 2 d S T P
O1 O 0.28576(6) 0.5000 0.0000 0.0337(4) Uani 1 4 d S T P
O4 O 0.31243(5) 0.41069(5) 0.05243(5) 0.0679(4) Uani 1 1 d . . .
C1 C 0.40397(11) 0.5000 0.0000 0.0548(9) Uani 1 4 d S T P
C4 C 0.16747(12) 0.5000 0.0000 0.0681(12) Uani 1 4 d S T P
O2 O 0.38510(6) 0.46300(7) 0.0000 0.0686(6) Uani 1 2 d S T P
O3 O 0.18636(6) 0.5000 0.03703(8) 0.0841(7) Uani 1 2 d S T P
O5 O 0.25901(5) 0.44724(5) 0.08885(5) 0.0693(4) Uani 1 1 d . . .
C9 C 0.28586(7) 0.41532(7) 0.08417(7) 0.0597(5) Uani 1 1 d . . .
C2 C 0.45384(11) 0.5000 0.0000 0.0606(10) Uani 1 4 d S T P
C13 C 0.28716(9) 0.31401(9) 0.18450(9) 0.0945(9) Uani 1 1 d . . .
C5 C 0.11783(13) 0.5000 0.0000 0.0902(17) Uani 1 4 d S T P
C14 C 0.25462(8) 0.34666(9) 0.18499(8) 0.0855(8) Uani 1 1 d . . .
C15 C 0.25440(8) 0.38023(8) 0.15247(8) 0.0838(8) Uani 1 1 d . . .
H15 H 0.2329 0.4026 0.1533 0.101 Uiso 1 1 calc R U .
C3 C 0.47683(9) 0.46073(11) 0.0000 0.0902(12) Uani 1 2 d S T P
H3 H 0.4614 0.4338 0.0000 0.108 Uiso 1 2 calc R U P
C8 C 0.02485(14) 0.5000 0.0000 0.126(3) Uani 1 4 d S T P
C11 C 0.31823(10) 0.34672(9) 0.11890(9) 0.1052(11) Uani 1 1 d . . .
H11 H 0.3395 0.3465 0.0963 0.126 Uiso 1 1 calc R U .
C10 C 0.28602(8) 0.37995(8) 0.11938(8) 0.0763(7) Uani 1 1 d . . .
C16 C 0.27829(9) 0.28315(9) 0.22372(9) 0.0928(9) Uani 1 1 d . . .
C12 C 0.31927(10) 0.31385(11) 0.15148(10) 0.1243(14) Uani 1 1 d . . .
H12 H 0.3413 0.2920 0.1511 0.149 Uiso 1 1 calc R U .
C6 C 0.09464(12) 0.5000 0.03796(16) 0.182(3) Uani 1 2 d S T P
H6 H 0.1097 0.5000 0.0651 0.218 Uiso 1 2 calc R U P
C7 C 0.04826(12) 0.5000 0.03765(18) 0.196(4) Uani 1 2 d S T P
H7 H 0.0331 0.5000 0.0647 0.235 Uiso 1 2 calc R U P
C17 C 0.24013(9) 0.29969(9) 0.24539(9) 0.0924(9) Uani 1 1 d . . .
C18 C 0.22212(9) 0.34178(9) 0.22261(9) 0.0969(10) Uani 1 1 d . . .
C19 C 0.17496(11) 0.33469(15) 0.20237(13) 0.1357(16) Uani 1 1 d . . .
H19A H 0.1536 0.3321 0.2266 0.163 Uiso 1 1 calc R U .
H19B H 0.1671 0.3610 0.1852 0.163 Uiso 1 1 calc R U .
C21 C 0.22377(15) 0.38357(12) 0.25234(12) 0.1314(16) Uani 1 1 d . . .
H21A H 0.2151 0.4092 0.2346 0.158 Uiso 1 1 calc R U .
H21B H 0.2020 0.3802 0.2761 0.158 Uiso 1 1 calc R U .
C22 C 0.2690(2) 0.39290(18) 0.27310(17) 0.199(2) Uani 1 1 d . . .
H22A H 0.2766 0.3692 0.2933 0.298 Uiso 1 1 calc R U .
H22B H 0.2678 0.4206 0.2892 0.298 Uiso 1 1 calc R U .
H22C H 0.2911 0.3948 0.2500 0.298 Uiso 1 1 calc R U .
C20 C 0.17024(17) 0.29329(19) 0.17190(19) 0.199(2) Uani 1 1 d . . .
H20A H 0.1921 0.2947 0.1485 0.299 Uiso 1 1 calc R U .
H20B H 0.1409 0.2928 0.1591 0.299 Uiso 1 1 calc R U .
H20C H 0.1748 0.2667 0.1892 0.299 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 109.10(10) . 14
O4 Zn1 O2 107.22(6) . .
O4 Zn1 O2 107.22(6) 14 .
O4 Zn1 O1 111.59(5) . .
O4 Zn1 O1 111.60(5) 14 .
O2 Zn1 O1 109.91(7) . .
O3 Zn2 O5 107.10(6) . .
O3 Zn2 O5 107.10(6) . 15_565
O5 Zn2 O5 109.52(10) . 15_565
O3 Zn2 O1 110.56(8) . .
O5 Zn2 O1 111.19(5) . .
O5 Zn2 O1 111.19(5) 15_565 .
Zn2 O1 Zn2 110.00(9) . 14
Zn2 O1 Zn1 109.037(6) . .
Zn2 O1 Zn1 109.035(6) 14 .
Zn2 O1 Zn1 109.038(6) . 15_565
Zn2 O1 Zn1 109.037(6) 14 15_565
Zn1 O1 Zn1 110.68(9) . 15_565
C9 O4 Zn1 131.34(13) . .
O2 C1 O2 125.9(3) . 15_565
O2 C1 C2 117.03(16) . .
O2 C1 C2 117.04(16) 15_565 .
O3 C4 O3 126.0(4) . 14
O3 C4 C5 117.02(18) . .
O3 C4 C5 117.02(18) 14 .
C1 O2 Zn1 131.77(19) . .
C4 O3 Zn2 131.5(2) . .
C9 O5 Zn2 131.47(13) . .
O4 C9 O5 125.29(17) . .
O4 C9 C10 117.18(18) . .
O5 C9 C10 117.53(18) . .
C3 C2 C3 119.3(4) 15_565 .
C3 C2 C1 120.34(18) 15_565 .
C3 C2 C1 120.34(18) . .
C12 C13 C14 120.1(2) . .
C12 C13 C16 132.4(2) . .
C14 C13 C16 107.44(19) . .
C6 C5 C6 117.2(5) . 14
C6 C5 C4 121.4(2) . .
C6 C5 C4 121.4(2) 14 .
C13 C14 C15 120.3(2) . .
C13 C14 C18 113.44(19) . .
C15 C14 C18 126.2(2) . .
C10 C15 C14 119.7(2) . .
C2 C3 C3 120.34(18) . 3_655
C7 C8 C7 116.3(5) . 14
C7 C8 C8 121.9(2) . 13_565
C7 C8 C8 121.9(2) 14 13_565
C10 C11 C12 121.2(2) . .
C15 C10 C11 119.5(2) . .
C15 C10 C9 120.2(2) . .
C11 C10 C9 120.24(19) . .
C17 C16 C17 119.9(2) 9 .
C17 C16 C13 133.5(2) 9 .
C17 C16 C13 106.57(19) . .
C13 C12 C11 119.1(2) . .
C5 C6 C7 121.0(4) . .
C8 C7 C6 122.3(5) . .
C16 C17 C16 120.1(2) 5 .
C16 C17 C18 128.1(2) 5 .
C16 C17 C18 111.78(19) . .
C14 C18 C17 100.77(18) . .
C14 C18 C21 109.6(3) . .
C17 C18 C21 113.6(3) . .
C14 C18 C19 108.1(3) . .
C17 C18 C19 112.5(3) . .
C21 C18 C19 111.5(3) . .
C20 C19 C18 115.0(3) . .
C22 C21 C18 114.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.9278(13) .
Zn1 O4 1.9279(13) 14
Zn1 O2 1.9327(17) .
Zn1 O1 1.9449(11) .
Zn2 O3 1.9253(19) .
Zn2 O5 1.9348(13) .
Zn2 O5 1.9349(13) 15_565
Zn2 O1 1.9400(11) .
O1 Zn2 1.9401(11) 14
O1 Zn1 1.9449(11) 15_565
O4 C9 1.247(2) .
C1 O2 1.244(2) .
C1 O2 1.244(2) 15_565
C1 C2 1.494(5) .
C4 O3 1.245(3) .
C4 O3 1.245(3) 14
C4 C5 1.487(5) .
O5 C9 1.257(2) .
C9 C10 1.495(3) .
C2 C3 1.363(4) 15_565
C2 C3 1.363(4) .
C13 C12 1.380(3) .
C13 C14 1.381(3) .
C13 C16 1.518(3) .
C5 C6 1.332(5) .
C5 C6 1.332(5) 14
C14 C15 1.400(3) .
C14 C18 1.496(3) .
C15 C10 1.371(3) .
C3 C3 1.388(5) 3_655
C8 C7 1.328(5) .
C8 C7 1.328(5) 14
C8 C8 1.489(8) 13_565
C11 C10 1.386(3) .
C11 C12 1.387(3) .
C16 C17 1.390(3) 9
C16 C17 1.405(3) .
C6 C7 1.389(5) .
C17 C16 1.390(3) 5
C17 C18 1.531(3) .
C18 C21 1.537(5) .
C18 C19 1.552(5) .
C19 C20 1.546(6) .
C21 C22 1.516(6) .
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 0.0 15_565 .
C2 C1 O2 Zn1 180.0 . .
O3 C4 O3 Zn2 0.0 14 .
C5 C4 O3 Zn2 180.0 . .
Zn1 O4 C9 O5 -1.4(4) . .
Zn1 O4 C9 C10 178.53(16) . .
Zn2 O5 C9 O4 -1.8(4) . .
Zn2 O5 C9 C10 178.28(16) . .
O2 C1 C2 C3 180.0 . 15_565
O2 C1 C2 C3 0.0 15_565 15_565
O2 C1 C2 C3 0.0 . .
O2 C1 C2 C3 180.0 15_565 .
O3 C4 C5 C6 0.0 . .
O3 C4 C5 C6 180.0 14 .
O3 C4 C5 C6 180.0 . 14
O3 C4 C5 C6 0.0 14 14
C12 C13 C14 C15 -1.1(5) . .
C16 C13 C14 C15 179.8(3) . .
C12 C13 C14 C18 179.3(3) . .
C16 C13 C14 C18 0.2(4) . .
C13 C14 C15 C10 1.6(5) . .
C18 C14 C15 C10 -178.8(3) . .
C3 C2 C3 C3 0.0 15_565 3_655
C1 C2 C3 C3 180.0 . 3_655
C14 C15 C10 C11 -0.9(5) . .
C14 C15 C10 C9 179.3(3) . .
C12 C11 C10 C15 -0.4(5) . .
C12 C11 C10 C9 179.3(3) . .
O4 C9 C10 C15 -172.7(2) . .
O5 C9 C10 C15 7.2(4) . .
O4 C9 C10 C11 7.5(4) . .
O5 C9 C10 C11 -172.5(3) . .
C12 C13 C16 C17 1.7(7) . 9
C14 C13 C16 C17 -179.3(4) . 9
C12 C13 C16 C17 -178.8(4) . .
C14 C13 C16 C17 0.2(4) . .
C14 C13 C12 C11 -0.3(6) . .
C16 C13 C12 C11 178.7(4) . .
C10 C11 C12 C13 1.0(6) . .
C6 C5 C6 C7 0.0 14 .
C4 C5 C6 C7 180.0 . .
C7 C8 C7 C6 0.0 14 .
C8 C8 C7 C6 180.0 13_565 .
C5 C6 C7 C8 0.0 . .
C17 C16 C17 C16 -0.1(7) 9 5
C13 C16 C17 C16 -179.7(3) . 5
C17 C16 C17 C18 179.0(2) 9 .
C13 C16 C17 C18 -0.5(4) . .
C13 C14 C18 C17 -0.5(4) . .
C15 C14 C18 C17 180.0(3) . .
C13 C14 C18 C21 119.6(3) . .
C15 C14 C18 C21 -60.0(4) . .
C13 C14 C18 C19 -118.6(3) . .
C15 C14 C18 C19 61.8(4) . .
C16 C17 C18 C14 179.7(3) 5 .
C16 C17 C18 C14 0.6(4) . .
C16 C17 C18 C21 62.6(5) 5 .
C16 C17 C18 C21 -116.5(3) . .
C16 C17 C18 C19 -65.3(5) 5 .
C16 C17 C18 C19 115.6(3) . .
C14 C18 C19 C20 59.4(4) . .
C17 C18 C19 C20 -51.0(4) . .
C21 C18 C19 C20 180.0(3) . .
C14 C18 C21 C22 -59.9(4) . .
C17 C18 C21 C22 52.0(4) . .
C19 C18 C21 C22 -179.6(3) . .
