#------------------------------------------------------------------------------
#$Date: 2019-11-25 04:51:04 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240048 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/92/4129298.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_4129298
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            'C59 H42 O13 Zn4'
_chemical_formula_weight         1220.40
_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                   29.9525(3)
_cell_length_b                   29.9525(3)
_cell_length_c                   29.9525(3)
_cell_measurement_reflns_used    35948
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.04
_cell_measurement_theta_min      6.61
_cell_volume                     26872.0(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 0.993
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            63191
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.032
_diffrn_reflns_theta_min         6.609
_diffrn_source                   'Rigaku MM007 rotating anode'
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.695629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.864
_exptl_crystal_size_mid          0.721
_exptl_crystal_size_min          0.633
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.029
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         9240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0292
_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)+(0.0327P)²+5.5884P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8556
_reflns_number_total             9240
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b00365_si_002.cif
_cod_data_source_block           MUF-77-Methyl
_cod_original_cell_volume        26872.0(8)
_cod_database_code               4129298
_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   0.556
_shelx_estimated_absorpt_t_max   0.642
_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 0.05332(2) 0.17736(2) 0.5000 0.03021(6) Uani 1 2 d S T P
Zn2 Zn 0.0000 0.25139(2) 0.44672(2) 0.03142(6) Uani 1 2 d S T P
O1 O 0.0000 0.21437(4) 0.5000 0.0276(3) Uani 1 4 d S T P
O5 O 0.05275(3) 0.24117(3) 0.41086(3) 0.0592(3) Uani 1 1 d . . .
O4 O 0.08913(3) 0.18763(3) 0.44736(3) 0.0596(3) Uani 1 1 d . . .
O2 O 0.03709(4) 0.11493(4) 0.5000 0.0600(4) Uani 1 2 d S T P
C1 C 0.0000 0.09604(7) 0.5000 0.0468(6) Uani 1 4 d S T P
C4 C 0.0000 0.33233(8) 0.5000 0.0558(7) Uani 1 4 d S T P
O3 O 0.0000 0.31367(4) 0.46293(5) 0.0713(4) Uani 1 2 d S T P
C9 C 0.08455(4) 0.21429(4) 0.41567(4) 0.0505(3) Uani 1 1 d . . .
C2 C 0.0000 0.04599(7) 0.5000 0.0524(6) Uani 1 4 d S T P
C15 C 0.11982(5) 0.24628(5) 0.34721(5) 0.0700(5) Uani 1 1 d . . .
H15 H 0.0976 0.2679 0.3464 0.084 Uiso 1 1 calc R U .
C13 C 0.18649(6) 0.21346(6) 0.31527(6) 0.0786(5) Uani 1 1 d . . .
C3 C 0.03933(7) 0.02314(6) 0.5000 0.0813(8) Uani 1 2 d S T P
H3 H 0.0662 0.0386 0.5000 0.098 Uiso 1 2 calc R U P
C14 C 0.15306(5) 0.24590(5) 0.31511(5) 0.0736(5) Uani 1 1 d . . .
C10 C 0.11991(5) 0.21426(5) 0.38049(5) 0.0637(4) Uani 1 1 d . . .
C11 C 0.15313(6) 0.18204(6) 0.38100(6) 0.0874(6) Uani 1 1 d . . .
H11 H 0.1533 0.1606 0.4034 0.105 Uiso 1 1 calc R U .
C17 C 0.20046(5) 0.26041(6) 0.25438(6) 0.0770(5) Uani 1 1 d . . .
C5 C 0.0000 0.38223(8) 0.5000 0.0758(10) Uani 1 4 d S T P
C16 C 0.21652(6) 0.22228(6) 0.27642(5) 0.0774(5) Uani 1 1 d . . .
C12 C 0.18609(6) 0.18132(6) 0.34861(6) 0.0994(8) Uani 1 1 d . . .
H12 H 0.2080 0.1593 0.3492 0.119 Uiso 1 1 calc R U .
C18 C 0.15846(6) 0.27862(6) 0.27712(6) 0.0821(6) Uani 1 1 d . . .
C20 C 0.11727(6) 0.27607(8) 0.24719(7) 0.1099(8) Uani 1 1 d . . .
H20A H 0.1120 0.2456 0.2389 0.165 Uiso 1 1 calc R U .
H20B H 0.1221 0.2936 0.2208 0.165 Uiso 1 1 calc R U .
H20C H 0.0918 0.2874 0.2630 0.165 Uiso 1 1 calc R U .
C19 C 0.16633(8) 0.32511(6) 0.29719(7) 0.1107(8) Uani 1 1 d . . .
H19A H 0.1397 0.3349 0.3122 0.166 Uiso 1 1 calc R U .
H19B H 0.1737 0.3457 0.2738 0.166 Uiso 1 1 calc R U .
H19C H 0.1905 0.3237 0.3182 0.166 Uiso 1 1 calc R U .
C8 C 0.0000 0.47509(9) 0.5000 0.1092(16) Uani 1 4 d S T P
C6 C 0.0000 0.40536(8) 0.46180(10) 0.162(2) Uani 1 2 d S T P
H6 H 0.0000 0.3902 0.4347 0.194 Uiso 1 2 calc R U P
C7 C 0.0000 0.45183(8) 0.46201(11) 0.180(2) Uani 1 2 d S T P
H7 H 0.0000 0.4671 0.4350 0.216 Uiso 1 2 calc R U P
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 109.42(6) 14_556 .
O4 Zn1 O2 107.09(4) 14_556 .
O4 Zn1 O2 107.09(4) . .
O4 Zn1 O1 111.43(3) 14_556 .
O4 Zn1 O1 111.43(3) . .
O2 Zn1 O1 110.19(5) . .
O3 Zn2 O5 107.03(4) . 16
O3 Zn2 O5 107.03(4) . .
O5 Zn2 O5 109.48(6) 16 .
O3 Zn2 O1 110.21(5) . .
O5 Zn2 O1 111.45(3) 16 .
O5 Zn2 O1 111.44(3) . .
Zn2 O1 Zn2 110.41(6) 14_556 .
Zn2 O1 Zn1 108.992(4) 14_556 3_556
Zn2 O1 Zn1 108.993(4) . 3_556
Zn2 O1 Zn1 108.990(4) 14_556 .
Zn2 O1 Zn1 108.991(4) . .
Zn1 O1 Zn1 110.46(6) 3_556 .
C9 O5 Zn2 131.09(8) . .
C9 O4 Zn1 131.43(8) . .
C1 O2 Zn1 131.58(12) . .
O2 C1 O2 126.0(2) 3_556 .
O2 C1 C2 117.00(10) 3_556 .
O2 C1 C2 117.00(10) . .
O3 C4 O3 126.6(2) . 14_556
O3 C4 C5 116.72(11) . .
O3 C4 C5 116.72(11) 14_556 .
C4 O3 Zn2 131.30(14) . .
O4 C9 O5 125.53(11) . .
O4 C9 C10 117.26(11) . .
O5 C9 C10 117.20(11) . .
C3 C2 C3 119.7(2) . 3_556
C3 C2 C1 120.16(11) . .
C3 C2 C1 120.16(11) 3_556 .
C10 C15 C14 119.57(13) . .
C12 C13 C14 118.66(13) . .
C12 C13 C16 133.51(13) . .
C14 C13 C16 107.82(12) . .
C2 C3 C3 120.16(11) . 15
C15 C14 C13 121.30(13) . .
C15 C14 C18 126.51(12) . .
C13 C14 C18 112.19(12) . .
C15 C10 C11 119.47(12) . .
C15 C10 C9 120.43(12) . .
C11 C10 C9 120.09(12) . .
C12 C11 C10 121.00(13) . .
C16 C17 C16 120.10(13) 9 .
C16 C17 C18 128.66(13) 9 .
C16 C17 C18 111.23(12) . .
C6 C5 C6 117.6(3) . 14_556
C6 C5 C4 121.19(14) . .
C6 C5 C4 121.19(14) 14_556 .
C17 C16 C17 119.90(13) 5 .
C17 C16 C13 132.42(13) 5 .
C17 C16 C13 107.68(12) . .
C11 C12 C13 119.99(14) . .
C14 C18 C20 108.87(16) . .
C14 C18 C17 101.07(11) . .
C20 C18 C17 112.64(16) . .
C14 C18 C19 108.05(15) . .
C20 C18 C19 113.54(16) . .
C17 C18 C19 111.79(16) . .
C7 C8 C7 117.0(3) 14_556 .
C7 C8 C8 121.48(15) 14_556 13_566
C7 C8 C8 121.48(15) . 13_566
C5 C6 C7 120.9(3) . .
C8 C7 C6 121.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.9315(8) 14_556
Zn1 O4 1.9315(8) .
Zn1 O2 1.9319(11) .
Zn1 O1 1.9441(7) .
Zn2 O3 1.9275(12) .
Zn2 O5 1.9349(8) 16
Zn2 O5 1.9350(8) .
Zn2 O1 1.9433(7) .
O1 Zn2 1.9432(7) 14_556
O1 Zn1 1.9441(7) 3_556
O5 C9 1.2553(15) .
O4 C9 1.2481(15) .
O2 C1 1.2467(15) .
C1 O2 1.2467(15) 3_556
C1 C2 1.499(3) .
C4 O3 1.2432(17) .
C4 O3 1.2434(17) 14_556
C4 C5 1.495(3) .
C9 C10 1.4941(17) .
C2 C3 1.362(2) .
C2 C3 1.362(2) 3_556
C15 C10 1.3833(18) .
C15 C14 1.3841(19) .
C13 C12 1.3870(19) .
C13 C14 1.3953(19) .
C13 C16 1.4945(18) .
C3 C3 1.386(3) 15
C14 C18 1.5105(18) .
C10 C11 1.3863(19) .
C11 C12 1.384(2) .
C17 C16 1.3939(19) 9
C17 C16 1.4041(18) .
C17 C18 1.5309(18) .
C5 C6 1.338(3) .
C5 C6 1.338(3) 14_556
C16 C17 1.3938(19) 5
C18 C20 1.527(3) .
C18 C19 1.535(3) .
C8 C7 1.334(3) 14_556
C8 C7 1.334(3) .
C8 C8 1.492(5) 13_566
C6 C7 1.392(3) .
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_556
Zn1 O2 C1 C2 180.0 . .
O3 C4 O3 Zn2 0.000(1) 14_556 .
C5 C4 O3 Zn2 180.000(0) . .
Zn1 O4 C9 O5 -1.8(2) . .
Zn1 O4 C9 C10 178.18(10) . .
Zn2 O5 C9 O4 -1.7(2) . .
Zn2 O5 C9 C10 178.31(10) . .
O2 C1 C2 C3 180.0 3_556 .
O2 C1 C2 C3 0.0 . .
O2 C1 C2 C3 0.0 3_556 3_556
O2 C1 C2 C3 180.0 . 3_556
C3 C2 C3 C3 0.0 3_556 15
C1 C2 C3 C3 180.0 . 15
C10 C15 C14 C13 0.8(3) . .
C10 C15 C14 C18 -178.88(19) . .
C12 C13 C14 C15 -0.3(3) . .
C16 C13 C14 C15 179.59(19) . .
C12 C13 C14 C18 179.4(2) . .
C16 C13 C14 C18 -0.7(2) . .
C14 C15 C10 C11 -0.5(3) . .
C14 C15 C10 C9 179.51(17) . .
O4 C9 C10 C15 -172.52(16) . .
O5 C9 C10 C15 7.4(2) . .
O4 C9 C10 C11 7.5(2) . .
O5 C9 C10 C11 -172.57(17) . .
C15 C10 C11 C12 -0.3(3) . .
C9 C10 C11 C12 179.7(2) . .
O3 C4 C5 C6 0.000(1) . .
O3 C4 C5 C6 180.000(1) 14_556 .
O3 C4 C5 C6 180.000(1) . 14_556
O3 C4 C5 C6 0.000(1) 14_556 14_556
C16 C17 C16 C17 0.1(4) 9 5
C18 C17 C16 C17 179.30(15) . 5
C16 C17 C16 C13 -179.97(16) 9 .
C18 C17 C16 C13 -0.8(2) . .
C12 C13 C16 C17 0.7(4) . 5
C14 C13 C16 C17 -179.2(2) . 5
C12 C13 C16 C17 -179.2(3) . .
C14 C13 C16 C17 0.9(2) . .
C10 C11 C12 C13 0.7(4) . .
C14 C13 C12 C11 -0.4(4) . .
C16 C13 C12 C11 179.7(2) . .
C15 C14 C18 C20 -61.3(3) . .
C13 C14 C18 C20 119.01(19) . .
C15 C14 C18 C17 179.9(2) . .
C13 C14 C18 C17 0.2(2) . .
C15 C14 C18 C19 62.4(3) . .
C13 C14 C18 C19 -117.26(19) . .
C16 C17 C18 C14 179.5(2) 9 .
C16 C17 C18 C14 0.3(2) . .
C16 C17 C18 C20 63.5(3) 9 .
C16 C17 C18 C20 -115.67(19) . .
C16 C17 C18 C19 -65.8(3) 9 .
C16 C17 C18 C19 115.07(19) . .
C6 C5 C6 C7 0.000(1) 14_556 .
C4 C5 C6 C7 180.000(1) . .
C7 C8 C7 C6 0.000(1) 14_556 .
C8 C8 C7 C6 180.000(1) 13_566 .
C5 C6 C7 C8 0.000(1) . .
