#------------------------------------------------------------------------------
#$Date: 2017-05-09 01:29:31 +0300 (Tue, 09 May 2017) $
#$Revision: 196559 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/58/4345862.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_4345862
loop_
_publ_author_name
'Dong, Jie'
'Xu, Hang'
'Hou, Sheng-Li'
'Wu, Zhi-Lei'
'Zhao, Bin'
_publ_section_title
;
 Metal--Organic Frameworks with Tb4 Clusters as Nodes: Luminescent
 Detection of Chromium(VI) and Chemical Fixation of CO2
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00323
_journal_year                    2017
_chemical_formula_moiety         '0.5(C96 H88 N16 O56 Tb8), 10(H2 O), H4 O'
_chemical_formula_sum            'C48 H68 N8 O39 Tb4'
_chemical_formula_weight         2016.78
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d'
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7100(4)
_cell_length_b                   21.7100(4)
_cell_length_c                   30.5654(12)
_cell_measurement_reflns_used    11592
_cell_measurement_temperature    122.15(10)
_cell_measurement_theta_max      28.8940
_cell_measurement_theta_min      3.1390
_cell_volume                     14406.2(7)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      122.15(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_measured_fraction_theta_max 0.9027
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   20.00   60.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000 -150.0000 40

#__ type_ start__ end____ width___ exp.time_
  2 omega   46.00   93.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372 -178.0000 -180.0000 47

#__ type_ start__ end____ width___ exp.time_
  3 omega   61.00   92.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372 -178.0000   90.0000 31

#__ type_ start__ end____ width___ exp.time_
  4 omega    1.00   32.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372    0.0000   90.0000 31
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0000871490
_diffrn_orient_matrix_UB_12      -0.0037462490
_diffrn_orient_matrix_UB_13      -0.0230614510
_diffrn_orient_matrix_UB_21      -0.0322510997
_diffrn_orient_matrix_UB_22      0.0051467003
_diffrn_orient_matrix_UB_23      -0.0003673003
_diffrn_orient_matrix_UB_31      0.0051892517
_diffrn_orient_matrix_UB_32      0.0320502517
_diffrn_orient_matrix_UB_33      -0.0026492517
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17191
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.004
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_min         3.253
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71091
_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    1.860
_exptl_crystal_description
;
;
_exptl_crystal_F_000             7872
_refine_diff_density_max         1.974
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3176
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0366
_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)+(0.0338P)²+268.0753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2623
_reflns_number_total             3176
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic7b00323_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        14406.2(8)
_cod_database_code               4345862
_chemical_oxdiff_formula         C1GD1
_chemical_oxdiff_usercomment     DJ-GD
_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 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H26A,H26B} of O26, All O(H) groups
 At 1.5 times of:
  {H22A,H22B} of O22, {H24A,H24B} of O24, {H23A,H23B} of O23, {H21A,H21B} of O21
2. Restrained distances
 O-H
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: H22A(0.5) H22B(0.5)
4.a Riding coordinates:
 O2(H2), O24(H24A,H24B), O26(H26A,H26B), O22(H22A,H22B), O(H)
4.b Rotating group:
 O21(H21A,H21B), O23(H23A,H23B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13)
;
_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+1/4, x+3/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'y+3/4, x+1/4, -z+1/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'y+5/4, x+3/4, -z+3/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'x-1/2, -y, z'
'-y-3/4, -x-1/4, z-1/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-y-1/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'
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
C3 C 0.7762(3) 0.5128(3) 0.43450(19) 0.0162(13) Uani 1 1 d . . .
C4 C 0.8051(3) 0.4590(3) 0.41987(19) 0.0156(13) Uani 1 1 d . . .
H4 H 0.7837 0.4219 0.4193 0.019 Uiso 1 1 calc R . .
C5 C 0.8657(3) 0.4614(3) 0.40627(19) 0.0161(13) Uani 1 1 d . . .
C6 C 0.8962(3) 0.5181(3) 0.4077(2) 0.0188(14) Uani 1 1 d . . .
H6 H 0.9370 0.5215 0.3989 0.023 Uiso 1 1 calc R . .
C7 C 0.8646(3) 0.5682(3) 0.4224(2) 0.0210(14) Uani 1 1 d . . .
H7 H 0.8854 0.6057 0.4235 0.025 Uiso 1 1 calc R . .
C9 C 0.7109(3) 0.5114(3) 0.44925(19) 0.0180(14) Uani 1 1 d . . .
C10 C 0.6762(3) 0.5647(3) 0.45391(19) 0.0159(13) Uani 1 1 d . . .
H10 H 0.6932 0.6028 0.4471 0.019 Uiso 1 1 calc R . .
C11 C 0.6164(3) 0.5608(3) 0.4687(2) 0.0188(14) Uani 1 1 d . . .
C12 C 0.5928(3) 0.5033(3) 0.4782(2) 0.0244(15) Uani 1 1 d . . .
H12 H 0.5523 0.4989 0.4876 0.029 Uiso 1 1 calc R . .
C13 C 0.6302(3) 0.4522(3) 0.4735(2) 0.0289(16) Uani 1 1 d . . .
H13 H 0.6142 0.4138 0.4808 0.035 Uiso 1 1 calc R . .
C15 C 0.5772(3) 0.6173(3) 0.4745(2) 0.0213(15) Uani 1 1 d . . .
C18 C 0.6549(3) 0.6475(3) 0.35929(19) 0.0158(13) Uani 1 1 d . . .
N8 N 0.8057(2) 0.5672(2) 0.43532(17) 0.0174(11) Uani 1 1 d . . .
N14 N 0.6880(2) 0.4551(2) 0.45914(19) 0.0227(13) Uani 1 1 d . . .
O2 O 0.49537(19) 0.81153(19) 0.40679(13) 0.0150(9) Uani 1 1 d . . .
H2 H 0.4975 0.8357 0.4175 0.018 Uiso 1 1 d R . .
O16 O 0.6037(2) 0.6686(2) 0.46899(15) 0.0229(10) Uani 1 1 d . . .
O17 O 0.5216(2) 0.6095(2) 0.48386(16) 0.0295(12) Uani 1 1 d . . .
O19 O 0.6250(2) 0.85360(19) 0.40135(15) 0.0211(10) Uani 1 1 d . . .
O20 O 0.66282(19) 0.6946(2) 0.38253(14) 0.0196(10) Uani 1 1 d . . .
O21 O 0.6874(2) 0.7655(2) 0.45776(15) 0.0259(11) Uani 1 1 d . . .
H21A H 0.6915 0.8025 0.4665 0.039 Uiso 1 1 d GR . .
H21B H 0.7165 0.7566 0.4401 0.039 Uiso 1 1 d GR . .
O23 O 0.5619(2) 0.8005(2) 0.48909(15) 0.0303(12) Uani 1 1 d . . .
H23A H 0.5573 0.7726 0.5090 0.045 Uiso 1 1 d GR . .
H23B H 0.5277 0.8207 0.4866 0.045 Uiso 1 1 d GR . .
Tb1 Tb 0.58850(2) 0.75395(2) 0.41997(2) 0.01429(13) Uani 1 1 d . . .
O24 O 0.7976(2) 0.6933(2) 0.45713(18) 0.0384(13) Uani 1 1 d . . .
H24A H 0.8139 0.6966 0.4823 0.058 Uiso 1 1 d R . .
H24B H 0.7958 0.6556 0.4499 0.058 Uiso 1 1 d R . .
O26 O 0.6059(4) 0.7679(4) 0.5709(2) 0.084(3) Uani 1 1 d . . .
H26A H 0.5937 0.7928 0.5905 0.101 Uiso 1 1 d R . .
H26B H 0.6372 0.7482 0.5801 0.101 Uiso 1 1 d R . .
O22 O 0.7500 0.8584(3) 0.5000 0.0173(13) Uani 1 2 d S T P
H22A H 0.7341 0.8882 0.5142 0.026 Uiso 0.5 1 d R . .
H22B H 0.7737 0.8726 0.4803 0.026 Uiso 0.5 1 d R . .
O O 0.5000 0.7500 0.6250 0.082(5) Uani 1 4 d DS T P
H H 0.4688 0.7725 0.6397 0.098 Uiso 1 1 d DR . .
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'
Tb Tb -0.1723 4.1537 '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
C4 C3 C9 120.4(6) . .
N8 C3 C4 121.8(6) . .
N8 C3 C9 117.8(5) . .
C5 C4 C3 119.5(6) . .
C4 C5 C6 118.3(6) . .
C4 C5 C18 120.5(6) . 15_445
C6 C5 C18 121.2(6) . 15_445
C7 C6 C5 118.4(6) . .
N8 C7 C6 124.4(6) . .
C10 C9 C3 122.0(6) . .
N14 C9 C3 115.9(6) . .
N14 C9 C10 122.0(6) . .
C11 C10 C9 119.5(6) . .
C10 C11 C12 118.3(6) . .
C10 C11 C15 121.5(6) . .
C12 C11 C15 120.2(6) . .
C11 C12 C13 119.1(6) . .
N14 C13 C12 123.3(7) . .
O16 C15 C11 116.4(6) . .
O17 C15 C11 117.5(6) . .
O17 C15 O16 126.0(6) . .
O19 C18 C5 117.9(5) 18_576 15_445
O20 C18 C5 116.5(5) . 15_445
O20 C18 O19 125.6(6) . 18_576
C7 N8 C3 117.6(5) . .
C13 N14 C9 117.6(6) . .
Tb1 O2 Tb1 107.95(16) 3_665 .
Tb1 O2 Tb1 108.56(16) 3_665 28_656
Tb1 O2 Tb1 106.42(15) . 28_656
C15 O16 Tb1 134.3(4) . .
C18 O19 Tb1 137.6(4) 28_656 .
C18 O20 Tb1 128.7(4) . .
O2 Tb1 O2 68.56(17) 3_665 .
O2 Tb1 O2 68.38(16) . 18_576
O2 Tb1 O2 69.45(16) 3_665 18_576
O2 Tb1 O16 75.34(15) 3_665 .
O2 Tb1 O19 140.44(14) 3_665 .
O2 Tb1 O20 96.70(14) 3_665 .
O2 Tb1 O21 131.98(15) 18_576 .
O2 Tb1 O21 145.41(15) 3_665 .
O2 Tb1 O21 139.49(14) . .
O2 Tb1 O23 74.24(15) . .
O2 Tb1 O23 102.65(16) 3_665 .
O2 Tb1 Tb1 36.36(10) 3_665 18_576
O2 Tb1 Tb1 36.73(10) 18_576 18_576
O2 Tb1 Tb1 76.02(10) 18_576 3_665
O2 Tb1 Tb1 36.86(9) . 28_656
O2 Tb1 Tb1 75.65(10) . 18_576
O2 Tb1 Tb1 36.60(10) 3_665 3_665
O2 Tb1 Tb1 76.27(10) 3_665 28_656
O2 Tb1 Tb1 35.45(10) . 3_665
O2 Tb1 Tb1 35.09(10) 18_576 28_656
O16 Tb1 O2 128.21(15) . .
O16 Tb1 O2 129.97(14) . 18_576
O16 Tb1 O21 70.42(16) . .
O16 Tb1 O23 79.06(15) . .
O16 Tb1 Tb1 95.91(11) . 3_665
O16 Tb1 Tb1 151.60(11) . 28_656
O16 Tb1 Tb1 96.22(11) . 18_576
O19 Tb1 O2 76.57(14) . .
O19 Tb1 O2 80.95(14) . 18_576
O19 Tb1 O16 143.65(15) . .
O19 Tb1 O21 74.15(15) . .
O19 Tb1 O23 84.70(16) . .
O19 Tb1 Tb1 64.56(10) . 28_656
O19 Tb1 Tb1 117.47(11) . 18_576
O19 Tb1 Tb1 112.00(10) . 3_665
O20 Tb1 O2 72.45(14) . 18_576
O20 Tb1 O2 140.82(14) . .
O20 Tb1 O16 77.75(15) . .
O20 Tb1 O19 98.78(15) . .
O20 Tb1 O21 71.67(15) . .
O20 Tb1 O23 144.77(15) . .
O20 Tb1 Tb1 72.34(10) . 18_576
O20 Tb1 Tb1 131.19(10) . 3_665
O20 Tb1 Tb1 105.61(10) . 28_656
O21 Tb1 Tb1 137.83(11) . 28_656
O21 Tb1 Tb1 143.51(10) . 18_576
O21 Tb1 Tb1 151.60(11) . 3_665
O23 Tb1 O2 142.11(15) . 18_576
O23 Tb1 O21 75.74(16) . .
O23 Tb1 Tb1 136.61(12) . 18_576
O23 Tb1 Tb1 77.28(12) . 3_665
O23 Tb1 Tb1 107.42(11) . 28_656
Tb1 Tb1 Tb1 60.177(4) 3_665 18_576
Tb1 Tb1 Tb1 59.646(9) 18_576 28_656
Tb1 Tb1 Tb1 60.177(4) 3_665 28_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C3 C4 1.400(8) .
C3 C9 1.488(9) .
C3 N8 1.343(8) .
C4 C5 1.380(9) .
C5 C6 1.398(9) .
C5 C18 1.485(8) 15_445
C6 C7 1.362(9) .
C7 N8 1.340(8) .
C9 C10 1.389(9) .
C9 N14 1.354(8) .
C10 C11 1.376(9) .
C11 C12 1.380(9) .
C11 C15 1.504(9) .
C12 C13 1.382(10) .
C13 N14 1.330(9) .
C15 O16 1.266(8) .
C15 O17 1.251(8) .
C18 C5 1.485(8) 15_445
C18 O19 1.260(7) 18_576
C18 O20 1.258(7) .
O2 Tb1 2.411(4) .
O2 Tb1 2.418(4) 28_656
O2 Tb1 2.345(4) 3_665
O16 Tb1 2.405(4) .
O19 C18 1.260(7) 28_656
O19 Tb1 2.374(4) .
O20 Tb1 2.361(4) .
O21 Tb1 2.450(4) .
O23 Tb1 2.412(4) .
Tb1 O2 2.418(4) 18_576
Tb1 O2 2.345(4) 3_665
Tb1 Tb1 3.8465(6) 3_665
Tb1 Tb1 3.8672(5) 28_656
Tb1 Tb1 3.8672(5) 18_576
