#------------------------------------------------------------------------------
#$Date: 2019-11-25 04:51:04 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240048 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/93/4129301.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_4129301
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            'C99 H122 O13 Zn4'
_chemical_formula_weight         1781.44
_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                   29.8614(5)
_cell_length_b                   29.8614(5)
_cell_length_c                   29.8614(5)
_cell_measurement_reflns_used    24542
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.00
_cell_measurement_theta_min      6.63
_cell_volume                     26627.5(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 0.996
_diffrn_measured_fraction_theta_max 0.986
_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  0.0543
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            84708
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.051
_diffrn_reflns_theta_min         6.630
_diffrn_source                   'Rigaku MM007 rotating anode'
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.571993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5640
_exptl_crystal_size_max          0.719
_exptl_crystal_size_mid          0.708
_exptl_crystal_size_min          0.615
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         9163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0786
_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)+(0.1446P)²+9.5742P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2480
_refine_ls_wR_factor_ref         0.2602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7044
_reflns_number_total             9163
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b00365_si_002.cif
_cod_data_source_block           MUF-77-Hexyl
_cod_original_cell_volume        26627.5(13)
_cod_database_code               4129301
_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   0.577
_shelx_estimated_absorpt_t_max   0.620
_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 0.44636(2) 0.32268(2) 0.0000 0.0641(2) Uani 1 2 d S T P
Zn2 Zn 0.5000 0.24864(2) 0.05292(2) 0.0682(2) Uani 1 2 d S T P
O1 O 0.5000 0.28610(11) 0.0000 0.0590(8) Uani 1 4 d S T P
O2 O 0.46292(13) 0.38503(10) 0.0000 0.1023(12) Uani 1 2 d S T P
O5 O 0.44674(11) 0.25901(11) 0.08824(10) 0.1131(10) Uani 1 1 d . . .
O4 O 0.41009(10) 0.31217(10) 0.05167(10) 0.1087(9) Uani 1 1 d . . .
O3 O 0.5000 0.18615(12) 0.03760(17) 0.1297(17) Uani 1 2 d S T P
C1 C 0.5000 0.4043(2) 0.0000 0.088(2) Uani 1 4 d S T P
C2 C 0.5000 0.4534(2) 0.0000 0.096(2) Uani 1 4 d S T P
C9 C 0.41461(15) 0.28612(15) 0.08276(15) 0.1028(13) Uani 1 1 d . . .
C4 C 0.5000 0.1675(3) 0.0000 0.116(3) Uani 1 4 d S T P
C13 C 0.3120(2) 0.2851(2) 0.1815(2) 0.154(3) Uani 1 1 d . . .
C3 C 0.4599(2) 0.47675(17) 0.0000 0.125(2) Uani 1 2 d S T P
H3 H 0.4329 0.4612 0.0000 0.150 Uiso 1 2 calc R U P
C14 C 0.34391(19) 0.25248(18) 0.1836(2) 0.141(2) Uani 1 1 d . . .
C5 C 0.5000 0.1181(3) 0.0000 0.166(6) Uani 1 4 d S T P
C15 C 0.37910(19) 0.25352(19) 0.15061(19) 0.143(2) Uani 1 1 d . . .
H15 H 0.4023 0.2328 0.1517 0.172 Uiso 1 1 calc R U .
C10 C 0.37810(19) 0.28509(18) 0.11775(18) 0.1326(19) Uani 1 1 d . . .
C11 C 0.3445(2) 0.3174(2) 0.1168(2) 0.166(3) Uani 1 1 d . . .
H11 H 0.3444 0.3389 0.0942 0.199 Uiso 1 1 calc R U .
C8 C 0.5000 0.0239(3) 0.0000 0.223(9) Uani 1 4 d S T P
C6 C 0.5000 0.0947(2) 0.0396(4) 0.254(8) Uani 1 2 d S T P
H6 H 0.5000 0.1095 0.0670 0.305 Uiso 1 2 calc R U P
C18 C 0.3393(2) 0.2201(2) 0.2196(2) 0.151(3) Uani 1 1 d . . .
C16 C 0.2797(2) 0.2766(2) 0.2216(2) 0.152(3) Uani 1 1 d . . .
C12 C 0.3111(3) 0.3178(2) 0.1492(2) 0.200(4) Uani 1 1 d . . .
H12 H 0.2888 0.3395 0.1490 0.240 Uiso 1 1 calc R U .
C17 C 0.29744(19) 0.2380(2) 0.2425(2) 0.144(2) Uani 1 1 d . . .
C7 C 0.5000 0.0475(3) 0.0375(4) 0.255(8) Uani 1 2 d S T P
H7 H 0.5000 0.0318 0.0644 0.306 Uiso 1 2 calc R U P
C23 C 0.3892(6) 0.2700(6) 0.2723(5) 0.366(10) Uani 1 1 d . . .
H23A H 0.3978 0.2910 0.2491 0.439 Uiso 1 1 calc R U .
H23B H 0.3615 0.2805 0.2857 0.439 Uiso 1 1 calc R U .
C22 C 0.3807(3) 0.2216(4) 0.2501(3) 0.214(5) Uani 1 1 d . . .
H22A H 0.4069 0.2133 0.2327 0.257 Uiso 1 1 calc R U .
H22B H 0.3772 0.1996 0.2737 0.257 Uiso 1 1 calc R U .
C19 C 0.3344(4) 0.1736(3) 0.2002(4) 0.215(5) Uani 1 1 d . . .
H19A H 0.3315 0.1524 0.2246 0.258 Uiso 1 1 calc R U .
H19B H 0.3616 0.1662 0.1840 0.258 Uiso 1 1 calc R U .
C20 C 0.2937(5) 0.1677(5) 0.1681(6) 0.314(8) Uani 1 1 d . . .
H20A H 0.2964 0.1898 0.1444 0.377 Uiso 1 1 calc R U .
H20B H 0.2667 0.1748 0.1848 0.377 Uiso 1 1 calc R U .
C21 C 0.2862(9) 0.1161(9) 0.1434(10) 0.61(2) Uiso 1 1 d . . .
H21A H 0.3120 0.1089 0.1256 0.908 Uiso 1 1 calc R U .
H21B H 0.2601 0.1169 0.1246 0.908 Uiso 1 1 calc R U .
H21C H 0.2822 0.0938 0.1662 0.908 Uiso 1 1 calc R U .
C24 C 0.4262 0.2689 0.3088 0.727 Uiso 1 1 d . U .
H24A H 0.4551 0.2666 0.2947 0.908 Uiso 1 1 calc R U .
H24B H 0.4217 0.2435 0.3279 0.908 Uiso 1 1 calc R U .
H24C H 0.4249 0.2958 0.3262 0.908 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 107.7(2) 14 .
O4 Zn1 O2 107.71(12) 14 .
O4 Zn1 O2 107.71(12) . .
O4 Zn1 O1 112.07(10) 14 .
O4 Zn1 O1 112.07(10) . .
O2 Zn1 O1 109.41(14) . .
O4 Zn1 Zn2 76.60(9) 14 14
O4 Zn1 Zn2 125.25(9) . 14
O2 Zn1 Zn2 123.16(10) . 14
O1 Zn1 Zn2 35.47(4) . 14
O4 Zn1 Zn2 125.25(9) 14 .
O4 Zn1 Zn2 76.60(9) . .
O2 Zn1 Zn2 123.16(10) . .
O1 Zn1 Zn2 35.47(4) . .
Zn2 Zn1 Zn2 60.12(2) 14 .
O3 Zn2 O5 106.58(12) . 16_655
O3 Zn2 O5 106.58(12) . .
O5 Zn2 O5 110.7(2) 16_655 .
O3 Zn2 O1 111.52(16) . .
O5 Zn2 O1 110.66(9) 16_655 .
O5 Zn2 O1 110.66(9) . .
O3 Zn2 Zn1 124.16(12) . 3_655
O5 Zn2 Zn1 75.13(8) 16_655 3_655
O5 Zn2 Zn1 125.37(9) . 3_655
O1 Zn2 Zn1 35.53(4) . 3_655
O3 Zn2 Zn1 124.16(12) . .
O5 Zn2 Zn1 125.37(9) 16_655 .
O5 Zn2 Zn1 75.13(8) . .
O1 Zn2 Zn1 35.53(4) . .
Zn1 Zn2 Zn1 61.03(2) 3_655 .
Zn2 O1 Zn2 109.41(16) 14 .
Zn2 O1 Zn1 108.997(12) 14 .
Zn2 O1 Zn1 108.998(12) . .
Zn2 O1 Zn1 108.996(12) 14 3_655
Zn2 O1 Zn1 108.997(12) . 3_655
Zn1 O1 Zn1 111.42(16) . 3_655
C1 O2 Zn1 132.4(4) . .
C9 O5 Zn2 130.9(3) . .
C9 O4 Zn1 131.1(3) . .
C4 O3 Zn2 130.2(5) . .
O2 C1 O2 125.0(6) . 3_655
O2 C1 C2 117.5(3) . .
O2 C1 C2 117.5(3) 3_655 .
C3 C2 C3 119.5(7) 3_655 .
C3 C2 C1 120.2(3) 3_655 .
C3 C2 C1 120.2(3) . .
O4 C9 O5 126.2(4) . .
O4 C9 C10 117.4(4) . .
O5 C9 C10 116.4(4) . .
O3 C4 O3 127.2(7) . 14
O3 C4 C5 116.4(4) . .
O3 C4 C5 116.4(4) 14 .
C14 C13 C12 123.6(5) . .
C14 C13 C16 106.4(4) . .
C12 C13 C16 130.0(5) . .
C2 C3 C3 120.2(3) . 15_565
C13 C14 C15 117.6(4) . .
C13 C14 C18 116.4(4) . .
C15 C14 C18 126.1(4) . .
C6 C5 C6 118.9(9) . 14
C6 C5 C4 120.5(5) . .
C6 C5 C4 120.5(5) 14 .
C10 C15 C14 119.5(5) . .
C15 C10 C11 120.7(4) . .
C15 C10 C9 119.8(5) . .
C11 C10 C9 119.4(4) . .
C12 C11 C10 120.5(5) . .
C7 C8 C7 115.7(11) 14 .
C7 C8 C8 122.2(5) 14 13_655
C7 C8 C8 122.2(5) . 13_655
C5 C6 C7 117.9(10) . .
C14 C18 C19 109.8(6) . .
C14 C18 C17 100.1(4) . .
C19 C18 C17 114.5(7) . .
C14 C18 C22 110.1(6) . .
C19 C18 C22 109.4(7) . .
C17 C18 C22 112.6(6) . .
C17 C16 C17 121.2(5) 5 .
C17 C16 C13 135.0(5) 5 .
C17 C16 C13 103.8(4) . .
C13 C12 C11 118.1(5) . .
C16 C17 C16 118.8(5) 9 .
C16 C17 C18 127.9(5) 9 .
C16 C17 C18 113.3(4) . .
C8 C7 C6 124.8(10) . .
C24 C23 C22 112.5(12) . .
C18 C22 C23 113.4(9) . .
C18 C19 C20 114.5(9) . .
C19 C20 C21 117.7(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.911(3) 14
Zn1 O4 1.911(3) .
Zn1 O2 1.926(3) .
Zn1 O1 1.9388(19) .
Zn1 Zn2 3.1545(6) 14
Zn1 Zn2 3.1545(6) .
Zn2 O3 1.921(4) .
Zn2 O5 1.933(3) 16_655
Zn2 O5 1.933(3) .
Zn2 O1 1.936(2) .
Zn2 Zn1 3.1545(6) 3_655
O1 Zn2 1.936(2) 14
O1 Zn1 1.9388(19) 3_655
O2 C1 1.248(5) .
O5 C9 1.266(5) .
O4 C9 1.219(5) .
O3 C4 1.253(5) .
C1 O2 1.248(5) 3_655
C1 C2 1.464(9) .
C2 C3 1.386(7) 3_655
C2 C3 1.386(7) .
C9 C10 1.511(6) .
C4 O3 1.253(5) 14
C4 C5 1.476(10) .
C13 C14 1.364(6) .
C13 C12 1.373(7) .
C13 C16 1.558(6) .
C3 C3 1.389(10) 15_565
C14 C15 1.441(6) .
C14 C18 1.451(6) .
C5 C6 1.374(10) .
C5 C6 1.374(10) 14
C15 C10 1.361(6) .
C10 C11 1.392(7) .
C11 C12 1.390(7) .
C8 C7 1.321(11) 14
C8 C7 1.321(11) .
C8 C8 1.430(19) 13_655
C6 C7 1.411(10) .
C18 C19 1.512(12) .
C18 C17 1.524(6) .
C18 C22 1.536(11) .
C16 C17 1.363(6) 5
C16 C17 1.415(6) .
C17 C16 1.363(6) 9
C23 C24 1.552(17) .
C23 C22 1.611(16) .
C19 C20 1.560(15) .
C20 C21 1.72(3) .
