#------------------------------------------------------------------------------
#$Date: 2019-11-23 11:51:41 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233176 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/86/4348608.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_4348608
loop_
_publ_author_name
'Chen, Di-Ming'
'Tian, Jia-Yue'
'Liu, Chun-Sen'
_publ_section_title
;
 Ligand Symmetry Modulation for Designing Mixed-Ligand Metal-Organic
 Frameworks: Gas Sorption and Luminescence Sensing Properties.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8892
_journal_page_last               8897
_journal_paper_doi               10.1021/acs.inorgchem.6b01419
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '0.33(C156 H102 N36 O24 Zn9)'
_chemical_formula_sum            'C52 H34 N12 O8 Zn3'
_chemical_formula_weight         1151.02
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.027(2)
_cell_length_b                   21.027(2)
_cell_length_c                   20.5274(10)
_cell_measurement_reflns_used    4197
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2660
_cell_measurement_theta_min      3.1890
_cell_volume                     7859.9(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2542
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   50.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7329  178.0000 -180.0000 28

#__ type_ start__ end____ width___ exp.time_
  2 omega  -83.00  -17.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8110  -57.0000 -180.0000 66

#__ type_ start__ end____ width___ exp.time_
  3 omega  -45.00   42.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8110   37.0000   30.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0326278000
_diffrn_orient_matrix_UB_12      -0.0050628000
_diffrn_orient_matrix_UB_13      0.0148661000
_diffrn_orient_matrix_UB_21      0.0006737000
_diffrn_orient_matrix_UB_22      -0.0256906000
_diffrn_orient_matrix_UB_23      0.0219575000
_diffrn_orient_matrix_UB_31      0.0212435000
_diffrn_orient_matrix_UB_32      0.0289002000
_diffrn_orient_matrix_UB_33      0.0221704000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.1394
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22578
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         3.180
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    0.730
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1752
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 1094 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         9152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0834
_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)+(0.0980P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2330
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4833
_reflns_number_total             9152
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01419_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        7859.6(16)
_cod_database_code               4348608
_chemical_oxdiff_formula         'C H O N Zn'
_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.
;
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a :
 N6(C1AA,N0AA,N8,C9)
2.b Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C11(H11), C15(H15), C16(H16), C19(H19), C21(H21), C22(H22),
 C23(H23), C26(H26), C33(H33), C34(H34), C3AA(H3AA), C5(H5), C2AA(H2AA), C2(H2)
2.c X=CH2 refined with riding coordinates:
 N12(H12A,H12B)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
'y, x, -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
Zn1 Zn 0.23710(8) 0.0000 0.8333 0.0617(5) Uani 1 2 d S T P
Zn2 Zn 0.06405(8) -0.16870(8) 0.60162(5) 0.0777(5) Uani 1 1 d . . .
O1 O 0.3131(5) 0.0372(5) 0.7667(3) 0.094(3) Uani 1 1 d . . .
N2 N 0.4146(5) 0.0927(6) 0.4234(3) 0.086(3) Uani 1 1 d . . .
O4 O 0.2388(5) 0.1368(5) 0.1558(4) 0.097(3) Uani 1 1 d . . .
N3 N 0.1504(3) -0.0741(3) 0.7814(2) 0.059(2) Uani 1 1 d . . .
C25 C 0.1574(3) -0.0816(3) 0.7166(2) 0.058(2) Uani 1 1 d G . .
H1AA H 0.2008 -0.0579 0.6928 0.070 Uiso 1 1 calc R . .
N4 N 0.0900(3) -0.1298(3) 0.6926(2) 0.059(2) Uani 1 1 d G . .
N5 N 0.0413(3) -0.1521(4) 0.7426(2) 0.059(2) Uani 1 1 d G . .
C26 C 0.0787(3) -0.1177(4) 0.7975(2) 0.065(3) Uani 1 1 d G . .
C2 C 0.3460(7) 0.0806(7) 0.6578(4) 0.080(3) Uani 1 1 d . . .
C1 C 0.3020(8) 0.0727(7) 0.7211(5) 0.087(4) Uani 1 1 d . . .
C9 C 0.5078(8) 0.0746(8) 0.4721(5) 0.098(4) Uani 1 1 d . . .
H11 H 0.5261 0.0642 0.5094 0.118 Uiso 1 1 calc R . .
N6 N 0.0506(6) -0.1234(6) 0.8557(3) 0.091(3) Uani 1 1 d . . .
H12A H 0.0042 -0.1511 0.8617 0.109 Uiso 1 1 calc R . .
H12B H 0.0786 -0.0994 0.8878 0.109 Uiso 1 1 calc R . .
N1 N 0.7316(5) 0.0599(5) 0.3975(3) 0.064(2) Uani 1 1 d . . .
C5 C 0.4126(7) 0.0843(7) 0.5407(5) 0.085(3) Uani 1 1 d . . .
C23 C 0.6837(7) 0.0263(8) 0.4418(5) 0.099(4) Uani 1 1 d . . .
H15 H 0.6932 -0.0010 0.4718 0.119 Uiso 1 1 calc R . .
C11 C 0.5048(8) 0.0862(7) 0.3595(4) 0.084(4) Uani 1 1 d . . .
H16 H 0.5218 0.0850 0.3180 0.101 Uiso 1 1 calc R . .
O3 O 0.3066(6) 0.1145(5) 0.0898(3) 0.115(3) Uani 1 1 d . . .
C12 C 0.4434(6) 0.0941(7) 0.3657(4) 0.076(3) Uani 1 1 d . . .
C22 C 0.7154(7) 0.0985(7) 0.3559(5) 0.081(4) Uani 1 1 d . . .
H19 H 0.7477 0.1212 0.3215 0.097 Uiso 1 1 calc R . .
O2 O 0.2616(7) 0.0981(6) 0.7217(4) 0.119(4) Uani 1 1 d . . .
C24 C 0.6198(9) 0.0272(8) 0.4488(5) 0.107(5) Uani 1 1 d . . .
H21 H 0.5861 -0.0010 0.4809 0.128 Uiso 1 1 calc R . .
C15 C 0.3821(8) 0.0992(9) 0.1934(4) 0.100(5) Uani 1 1 d . . .
H22 H 0.3956 0.0960 0.1509 0.120 Uiso 1 1 calc R . .
C19 C 0.3419(8) 0.1035(10) 0.3189(5) 0.114(5) Uani 1 1 d . . .
H23 H 0.3261 0.1043 0.3611 0.136 Uiso 1 1 calc R . .
C8 C 0.4490(7) 0.0838(7) 0.4774(4) 0.085(4) Uani 1 1 d . . .
C10 C 0.5420(6) 0.0800(7) 0.4132(4) 0.078(3) Uani 1 1 d . . .
C3 C 0.3949(9) 0.0550(9) 0.6551(5) 0.114(5) Uani 1 1 d . . .
H26 H 0.4041 0.0352 0.6920 0.137 Uiso 1 1 calc R . .
C17 C 0.2866(8) 0.1191(8) 0.1457(6) 0.089(3) Uani 1 1 d . . .
C20 C 0.6053(7) 0.0718(7) 0.4065(4) 0.078(3) Uani 1 1 d . . .
C16 C 0.3246(7) 0.1090(7) 0.2030(5) 0.079(3) Uani 1 1 d . . .
C13 C 0.4033(8) 0.0979(8) 0.3080(4) 0.088(4) Uani 1 1 d . . .
C14 C 0.4225(9) 0.0934(10) 0.2447(5) 0.125(6) Uani 1 1 d . . .
H33 H 0.4622 0.0867 0.2363 0.150 Uiso 1 1 calc R . .
C21 C 0.6594(7) 0.1071(7) 0.3592(5) 0.087(4) Uani 1 1 d . . .
H34 H 0.6546 0.1377 0.3292 0.105 Uiso 1 1 calc R . .
C4 C 0.4309(8) 0.0589(9) 0.5957(4) 0.118(6) Uani 1 1 d . . .
H3AA H 0.4662 0.0447 0.5936 0.141 Uiso 1 1 calc R . .
C7 C 0.3345(12) 0.1066(10) 0.6044(5) 0.153(9) Uani 1 1 d . . .
H5 H 0.3041 0.1270 0.6070 0.184 Uiso 1 1 calc R . .
C6 C 0.3639(10) 0.1065(12) 0.5435(5) 0.149(8) Uani 1 1 d . . .
H2AA H 0.3498 0.1215 0.5063 0.179 Uiso 1 1 calc R . .
C18 C 0.3021(8) 0.1082(9) 0.2629(6) 0.112(5) Uani 1 1 d . . .
H2 H 0.2597 0.1107 0.2696 0.134 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
O1 Zn1 O1 103.4(5) . 4_556
O1 Zn1 N3 100.6(3) 4_556 4_556
O1 Zn1 N3 100.6(3) . .
O1 Zn1 N3 117.4(3) 4_556 .
O1 Zn1 N3 117.4(3) . 4_556
N3 Zn1 N3 117.5(4) . 4_556
O4 Zn2 N5 100.7(5) 4 5_556
O4 Zn2 N1 99.0(3) 4 6_546
O4 Zn2 O3 58.6(3) 4 4
O4 Zn2 C17 29.6(3) 4 4
N4 Zn2 O4 138.4(4) . 4
N4 Zn2 N5 104.4(4) . 5_556
N4 Zn2 N1 105.9(3) . 6_546
N4 Zn2 O3 89.5(2) . 4
N4 Zn2 C17 116.3(3) . 4
N5 Zn2 N1 104.9(6) 5_556 6_546
N5 Zn2 O3 157.9(5) 5_556 4
N5 Zn2 C17 130.2(5) 5_556 4
N1 Zn2 O3 87.2(4) 6_546 4
N1 Zn2 C17 90.9(4) 6_546 4
O3 Zn2 C17 29.2(3) 4 4
C1 O1 Zn1 113.2(8) . .
C12 N2 C8 117.1(9) . .
C17 O4 Zn2 98.1(8) . 4
C25 N3 Zn1 120.0(3) . .
C25 N3 C26 108.0 . .
C26 N3 Zn1 131.7(3) . .
N3 C25 N4 108.0 . .
C25 N4 Zn2 127.8(3) . .
C25 N4 N5 108.0 . .
N5 N4 Zn2 124.1(3) . .
N4 N5 Zn2 121.8(3) . 5_556
C26 N5 Zn2 129.7(3) . 5_556
C26 N5 N4 108.0 . .
N5 C26 N3 108.0 . .
N6 C26 N3 125.5(6) . .
N6 C26 N5 126.4(6) . .
C3 C2 C1 120.7(10) . .
C7 C2 C1 121.6(13) . .
C7 C2 C3 117.5(11) . .
O1 C1 C2 113.6(12) . .
O2 C1 O1 128.1(11) . .
O2 C1 C2 118.2(12) . .
C8 C9 C10 122.4(11) . .
C23 N1 Zn2 121.7(7) . 6_656
C23 N1 C22 114.9(9) . .
C22 N1 Zn2 123.0(7) . 6_656
C4 C5 C8 117.3(11) . .
C6 C5 C8 121.7(10) . .
C6 C5 C4 121.0(10) . .
N1 C23 C24 125.5(11) . .
C12 C11 C10 122.6(9) . .
C17 O3 Zn2 80.4(8) . 4
N2 C12 C11 121.4(9) . .
N2 C12 C13 116.9(10) . .
C11 C12 C13 121.6(9) . .
C21 C22 N1 125.8(10) . .
C23 C24 C20 118.9(11) . .
C16 C15 C14 122.5(10) . .
C13 C19 C18 118.3(10) . .
N2 C8 C5 112.7(11) . .
C9 C8 N2 122.1(9) . .
C9 C8 C5 125.2(10) . .
C9 C10 C11 114.0(11) . .
C9 C10 C20 123.4(10) . .
C11 C10 C20 122.3(8) . .
C2 C3 C4 119.5(11) . .
O4 C17 Zn2 52.3(6) . 4
O4 C17 C16 118.5(11) . .
O3 C17 Zn2 70.4(7) . 4
O3 C17 O4 122.0(12) . .
O3 C17 C16 119.3(12) . .
C16 C17 Zn2 164.2(9) . 4
C24 C20 C10 122.7(10) . .
C21 C20 C24 113.1(11) . .
C21 C20 C10 124.2(10) . .
C15 C16 C17 119.6(10) . .
C18 C16 C15 118.8(11) . .
C18 C16 C17 121.6(12) . .
C19 C13 C12 117.5(9) . .
C19 C13 C14 118.7(11) . .
C14 C13 C12 123.8(11) . .
C13 C14 C15 119.6(11) . .
C22 C21 C20 121.6(11) . .
C5 C4 C3 118.8(12) . .
C2 C7 C6 125.3(14) . .
C5 C6 C7 117.5(12) . .
C16 C18 C19 121.8(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.945(7) .
Zn1 O1 1.945(7) 4_556
Zn1 N3 2.012(5) .
Zn1 N3 2.012(5) 4_556
Zn2 O4 2.005(7) 4
Zn2 N4 2.002(4) .
Zn2 N5 2.020(14) 5_556
Zn2 N1 2.053(8) 6_546
Zn2 O3 2.396(10) 4
Zn2 C17 2.508(13) 4
O1 C1 1.289(15) .
N2 C12 1.324(11) .
N2 C8 1.387(13) .
O4 Zn2 2.005(7) 4
O4 C17 1.251(14) .
N3 C25 1.357(4) .
N3 C26 1.357(4) .
C25 N4 1.357(4) .
N4 N5 1.357(4) .
N5 Zn2 2.020(6) 5_556
N5 C26 1.357(4) .
C26 N6 1.311(8) .
C2 C1 1.555(14) .
C2 C3 1.381(17) .
C2 C7 1.301(15) .
C1 O2 1.209(15) .
C9 C8 1.349(16) .
C9 C10 1.382(13) .
N1 Zn2 2.053(8) 6_656
N1 C23 1.277(13) .
N1 C22 1.336(12) .
C5 C8 1.511(13) .
C5 C4 1.383(15) .
C5 C6 1.322(17) .
C23 C24 1.361(17) .
C11 C12 1.389(15) .
C11 C10 1.394(14) .
O3 Zn2 2.396(10) 4
O3 C17 1.242(13) .
C12 C13 1.478(14) .
C22 C21 1.280(15) .
C24 C20 1.419(15) .
C15 C16 1.339(15) .
C15 C14 1.397(15) .
C19 C13 1.373(16) .
C19 C18 1.452(16) .
C10 C20 1.433(15) .
C3 C4 1.416(14) .
C17 Zn2 2.508(13) 4
C17 C16 1.496(16) .
C20 C21 1.393(14) .
C16 C18 1.315(15) .
C13 C14 1.378(14) .
C7 C6 1.394(14) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.099 -0.090 -0.014 4988 511 ' '
