#------------------------------------------------------------------------------
#$Date: 2020-08-05 04:20:29 +0300 (Wed, 05 Aug 2020) $
#$Revision: 254818 $
#$URL: svn://www.crystallography.net/cod/cif/1/55/87/1558782.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_1558782
loop_
_publ_author_name
'Zeng, Min'
'Ren, Ang'
'Wu, Wubin'
'Zhao, Yong Sheng'
'Zhan, Chuanlang'
'Yao, Jiannian'
_publ_section_title
;
 Lanthanide MOFs for Inducing Molecular Chirality of Achiral Stilbazolium
 with Strong Circularly Polarized Luminescence and Efficient Energy
 Transfer for Color Tuning
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02856H
_journal_year                    2020
_chemical_formula_moiety         '0.25(C36 H20 O28 Tb4)'
_chemical_formula_sum            'C9 H5 O7 Tb'
_chemical_formula_weight         384.05
_space_group_crystal_system      tetragonal
_space_group_IT_number           95
_space_group_name_Hall           'P 4cw 2c'
_space_group_name_H-M_alt        'P 43 2 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-18 deposited with the CCDC.	2020-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2191(2)
_cell_length_b                   10.2191(2)
_cell_length_c                   14.3738(5)
_cell_measurement_reflns_used    4119
_cell_measurement_temperature    169.97(10)
_cell_measurement_theta_max      73.6750
_cell_measurement_theta_min      3.0040
_cell_volume                     1501.06(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     11.00  91.00   0.50    0.13    --   46.95-117.00  78.00  160
  2  ω   -168.00 -86.00   0.50    0.53    --  -99.00 -45.00 150.00  164
  3  ω     82.00 169.00   0.50    0.53    --  103.25 117.00 166.00  174
  4  ω     32.00 116.00   0.50    0.53    --  103.25 -45.00 150.00  168
  5  ω   -119.00 -71.00   0.50    0.13    --  -46.95-125.00-120.00   96
  6  ω     34.00 119.00   0.50    0.13    --   46.95  45.00 -59.00  170
  7  ω   -168.00 -86.00   0.50    0.53    --  -99.00 -45.00   0.00  164
  8  ω     91.00 169.00   0.50    0.53    --  103.25  45.00-180.00  156
  9  ω     32.00  92.00   0.50    0.13    --   46.95  57.00  60.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0626153000
_diffrn_orient_matrix_UB_12      0.1118369000
_diffrn_orient_matrix_UB_13      0.0563954000
_diffrn_orient_matrix_UB_21      -0.0564280000
_diffrn_orient_matrix_UB_22      0.0584394000
_diffrn_orient_matrix_UB_23      -0.0902703000
_diffrn_orient_matrix_UB_31      -0.1250730000
_diffrn_orient_matrix_UB_32      -0.0823723000
_diffrn_orient_matrix_UB_33      0.0125045000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7117
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.165
_diffrn_reflns_theta_min         4.326
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       needle
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1490
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0536
_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)+(0.0218P)²+15.9645P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.599
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                1446
_reflns_number_total             1490
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc02856h2.cif
_cod_data_source_block           tx1606-a_sq
_cod_original_cell_volume        1501.06(8)
_cod_database_code               1558782
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         TbCHO
_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 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(3)
 0.11(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
O3A \\sim O3 \\sim O2 \\sim O2A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O2) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O2A)=Sof(O3A)=1-FVAR(1)
 Sof(O2)=Sof(O3)=FVAR(1)
 Fixed Sof: O4(0.5) H4A(0.5) H4B(0.5)
5.a Riding coordinates:
 O4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.653
_oxdiff_exptl_absorpt_empirical_full_min 0.573
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+3/4'
'-x, -y, z+1/2'
'y, -x, z+1/4'
'x, -y, -z+1/2'
'-x, y, -z'
'y, x, -z+1/4'
'-y, -x, -z+3/4'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.14509(7) 0.85491(7) 0.375000 0.0361(3) Uani 1 2 d S T P . .
O1 O 0.0745(11) 0.8979(17) 0.5909(13) 0.117(7) Uani 1 1 d . . . . .
O2 O 0.233(3) 0.933(3) 0.5154(18) 0.060(7) Uani 0.53(4) 1 d . U . A 1
O3 O 0.331(2) 0.901(3) 0.2997(17) 0.046(6) Uani 0.53(4) 1 d . U . A 1
O4 O 0.323(5) 0.701(4) 0.347(2) 0.123(15) Uani 0.5 1 d . . . A .
H4A H 0.383278 0.663898 0.378441 0.185 Uiso 0.5 1 d R . . . .
H4B H 0.337638 0.684708 0.290291 0.185 Uiso 0.5 1 d R . . . .
C1 C 0.467(2) 1.000000 0.750000 0.063(7) Uani 1 2 d S T P . .
C2 C 0.3985(13) 0.9593(17) 0.6709(9) 0.048(4) Uani 1 1 d . . . . .
H2 H 0.442990 0.931171 0.618114 0.057 Uiso 1 1 calc R . . . .
C3 C 0.2638(14) 0.9617(16) 0.6728(10) 0.047(4) Uani 1 1 d . . . . .
C4 C 0.1974(19) 1.000000 0.750000 0.050(5) Uani 1 2 d S T P . .
H4 H 0.106372 0.999999 0.750001 0.060 Uiso 1 2 calc RS T P . .
C5 C 0.1904(17) 0.915(2) 0.5879(12) 0.063(5) Uani 1 1 d . . . . .
C6 C 0.385(2) 1.000000 0.250000 0.067(7) Uani 1 2 d S T P . .
O2A O 0.270(3) 0.879(4) 0.509(2) 0.063(8) Uani 0.47(4) 1 d . U . A 2
O3A O 0.331(2) 0.965(3) 0.3228(18) 0.039(6) Uani 0.47(4) 1 d . U . A 2
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'
Tb Tb -9.1472 9.1891 '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
_geom_angle_publ_flag
O1 Tb1 O1 71.5(8) 2_664 6_556 ?
O1 Tb1 O2 97.0(10) 6_556 . ?
O1 Tb1 O2 97.0(10) 2_664 8_665 ?
O1 Tb1 O2 85.6(10) 2_664 . ?
O1 Tb1 O2 85.6(10) 6_556 8_665 ?
O1 Tb1 O4 136.5(11) 2_664 . ?
O1 Tb1 O4 150.6(14) 2_664 8_665 ?
O1 Tb1 O4 136.5(11) 6_556 8_665 ?
O1 Tb1 O4 150.6(14) 6_556 . ?
O2 Tb1 O2 176.8(19) . 8_665 ?
O2 Tb1 O4 94.4(16) . . ?
O2 Tb1 O4 94.4(16) 8_665 8_665 ?
O2 Tb1 O4 82.5(16) . 8_665 ?
O2 Tb1 O4 82.5(16) 8_665 . ?
O3 Tb1 O1 81.8(9) . 2_664 ?
O3 Tb1 O1 151.4(8) . 6_556 ?
O3 Tb1 O1 151.4(8) 8_665 2_664 ?
O3 Tb1 O1 81.8(9) 8_665 6_556 ?
O3 Tb1 O2 91.2(11) . . ?
O3 Tb1 O2 87.4(9) . 8_665 ?
O3 Tb1 O2 87.4(9) 8_665 . ?
O3 Tb1 O2 91.2(11) 8_665 8_665 ?
O3 Tb1 O3 126.1(15) . 8_665 ?
O3 Tb1 O4 54.7(13) 8_665 8_665 ?
O3 Tb1 O4 54.7(13) . . ?
O3 Tb1 O4 71.7(12) . 8_665 ?
O3 Tb1 O4 71.7(12) 8_665 . ?
O3 Tb1 O2A 78.7(10) . 8_665 ?
O3 Tb1 O2A 85.0(11) 8_665 8_665 ?
O3 Tb1 O3A 18.4(6) 8_665 8_665 ?
O3 Tb1 O3A 137.3(12) . 8_665 ?
O4 Tb1 O4 20.5(13) . 8_665 ?
O2A Tb1 O1 109.4(10) . 6_556 ?
O2A Tb1 O1 100.0(11) 8_665 6_556 ?
O2A Tb1 O4 65.8(16) 8_665 . ?
O2A Tb1 O4 78.2(16) . . ?
O2A Tb1 O3A 94.9(10) . 8_665 ?
O2A Tb1 O3A 76.6(10) 8_665 8_665 ?
O2A Tb1 O3A 76.6(10) . . ?
O2A Tb1 O3A 94.9(10) 8_665 . ?
O3A Tb1 O1 139.4(8) . 6_556 ?
O3A Tb1 O1 67.9(8) 8_665 6_556 ?
O3A Tb1 O4 83.4(13) 8_665 . ?
O3A Tb1 O4 69.6(14) . . ?
O3A Tb1 O3A 152.8(14) . 8_665 ?
C5 O1 Tb1 169.6(17) . 4_465 ?
C5 O2 Tb1 126(2) . . ?
C6 O3 Tb1 139(2) . . ?
O4 O4 Tb1 79.8(6) 8_665 . ?
C2 C1 C2 119.9(19) 5_576 . ?
C2 C1 C6 120.1(10) 5_576 3_675 ?
C2 C1 C6 120.1(10) . 3_675 ?
C3 C2 C1 118.6(15) . . ?
C2 C3 C5 118.3(15) . . ?
C4 C3 C2 121.4(15) . . ?
C4 C3 C5 120.2(14) . . ?
C3 C4 C3 120.0(19) 5_576 . ?
O1 C5 C3 120.5(18) . . ?
O1 C5 O2A 123(2) . . ?
O2 C5 O1 115(2) . . ?
O2 C5 C3 120(2) . . ?
O2A C5 C3 115.9(17) . . ?
O3 C6 O3 132(3) 5_575 . ?
O3 C6 C1 113.8(13) 5_575 3_674 ?
O3 C6 C1 113.8(13) . 3_674 ?
O3A C6 O3 119.0(19) . 5_575 ?
O3A C6 O3 32.6(12) 5_575 5_575 ?
O3A C6 O3A 127(3) 5_575 . ?
C5 O2A Tb1 111.7(19) . . ?
C6 O3A Tb1 141(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.339(13) 6_556 ?
Tb1 O1 2.339(13) 2_664 ?
Tb1 O2 2.35(2) 8_665 ?
Tb1 O2 2.35(2) . ?
Tb1 O3 2.24(2) 8_665 ?
Tb1 O3 2.24(2) . ?
Tb1 O4 2.44(2) . ?
Tb1 O4 2.44(2) 8_665 ?
Tb1 O2A 2.32(3) . ?
Tb1 O2A 2.32(3) 8_665 ?
Tb1 O3A 2.33(2) . ?
Tb1 O3A 2.33(2) 8_665 ?
O1 C5 1.20(2) . ?
O2 C5 1.14(3) . ?
O3 C6 1.36(3) . ?
O4 O4 0.87(5) 8_665 ?
C1 C2 1.399(16) 5_576 ?
C1 C2 1.399(16) . ?
C1 C6 1.52(3) 3_675 ?
C2 C3 1.377(19) . ?
C3 C4 1.358(18) . ?
C3 C5 1.51(2) . ?
C5 O2A 1.44(4) . ?
C6 O3A 1.23(2) . ?
C6 O3A 1.23(2) 5_575 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.89(3)
2 0.11(3)
