#------------------------------------------------------------------------------
#$Date: 2024-06-13 00:42:23 +0200 (Thu 13 de Jun de 2024) $
#$Revision: 292327 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/88/7248841.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_7248841
loop_
_publ_author_name
'Cao, Wenqian'
'Teng, Fangying'
'Cui, Yuanjing'
'Qian, Guodong'
_publ_section_title
;
 A Lanthanide Metal-organic Framework Containing Hydrazine Group for
 Highly Sensitive Luminescent Sensing of Formaldehyde Gas
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D4CE00406J
_journal_year                    2024
_chemical_formula_moiety         'C96 H48 O67 Tb12'
_chemical_formula_sum            'C96 H48 O67 Tb12'
_chemical_formula_weight         4180.38
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-16 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.5579(5)
_cell_length_b                   21.5579(5)
_cell_length_c                   21.5579(5)
_cell_measurement_reflns_used    3731
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      67.144
_cell_measurement_theta_min      3.551
_cell_volume                     10018.9(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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_temperature      299.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8735
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.969
_diffrn_reflns_theta_min         3.551
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.869
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1013 before and 0.0849 after correction. The Ratio of minimum to maximum transmission is 0.7093. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.289
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         513
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0693
_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)+(0.1231P)²+293.5249P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                462
_reflns_number_total             513
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00406j2.cif
_cod_data_source_block           cu_20230606tfy_tb_115k_0m_a_pl_sq
_cod_original_cell_volume        10018.9(7)
_cod_database_code               7248841
_shelx_shelxl_version_number     2016/6
_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_max   0.573
_shelx_estimated_absorpt_t_min   0.489
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C005-C004 = C1-C005
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C005) \\sim Ueq, Uanis(C004) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O1(0.03125)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'y, x, -z'
'-x, y, -z'
'-y, -x, -z'
'z, x, y'
'-x, z, y'
'-z, -x, y'
'x, -z, y'
'z, -x, -y'
'x, z, -y'
'-z, x, -y'
'-x, -z, -y'
'y, z, x'
'-z, -y, -x'
'-z, y, x'
'z, y, -x'
'z, -y, x'
'y, -z, -x'
'-y, -z, x'
'-y, z, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -y+1/2, -z+1/2'
'y, x+1/2, -z+1/2'
'-x, y+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'-x, z+1/2, y+1/2'
'-z, -x+1/2, y+1/2'
'x, -z+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'x, z+1/2, -y+1/2'
'-z, x+1/2, -y+1/2'
'-x, -z+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'-z, y+1/2, x+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -y, -z+1/2'
'y+1/2, x, -z+1/2'
'-x+1/2, y, -z+1/2'
'-y+1/2, -x, -z+1/2'
'z+1/2, x, y+1/2'
'-x+1/2, z, y+1/2'
'-z+1/2, -x, y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, -x, -y+1/2'
'x+1/2, z, -y+1/2'
'-z+1/2, x, -y+1/2'
'-x+1/2, -z, -y+1/2'
'y+1/2, z, x+1/2'
'-z+1/2, -y, -x+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'-y+1/2, z, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -y+1/2, -z'
'y+1/2, x+1/2, -z'
'-x+1/2, y+1/2, -z'
'-y+1/2, -x+1/2, -z'
'z+1/2, x+1/2, y'
'-x+1/2, z+1/2, y'
'-z+1/2, -x+1/2, y'
'x+1/2, -z+1/2, y'
'z+1/2, -x+1/2, -y'
'x+1/2, z+1/2, -y'
'-z+1/2, x+1/2, -y'
'-x+1/2, -z+1/2, -y'
'y+1/2, z+1/2, x'
'-z+1/2, -y+1/2, -x'
'-z+1/2, y+1/2, x'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z'
'-y, -x, z'
'x, -y, z'
'y, x, z'
'-z, -x, -y'
'x, -z, -y'
'z, x, -y'
'-x, z, -y'
'-z, x, y'
'-x, -z, y'
'z, -x, y'
'x, z, y'
'-y, -z, -x'
'z, y, x'
'z, -y, -x'
'-z, -y, x'
'-z, y, -x'
'-y, z, x'
'y, z, -x'
'y, -z, x'
'-x, -y+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-x, y+1/2, z+1/2'
'-y, -x+1/2, z+1/2'
'x, -y+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'x, -z+1/2, -y+1/2'
'z, x+1/2, -y+1/2'
'-x, z+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'-x, -z+1/2, y+1/2'
'z, -x+1/2, y+1/2'
'x, z+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'z, -y+1/2, -x+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'y+1/2, -x, -z+1/2'
'x+1/2, y, -z+1/2'
'-y+1/2, x, -z+1/2'
'-x+1/2, y, z+1/2'
'-y+1/2, -x, z+1/2'
'x+1/2, -y, z+1/2'
'y+1/2, x, z+1/2'
'-z+1/2, -x, -y+1/2'
'x+1/2, -z, -y+1/2'
'z+1/2, x, -y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, x, y+1/2'
'-x+1/2, -z, y+1/2'
'z+1/2, -x, y+1/2'
'x+1/2, z, y+1/2'
'-y+1/2, -z, -x+1/2'
'z+1/2, y, x+1/2'
'z+1/2, -y, -x+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'y+1/2, -z, x+1/2'
'-x+1/2, -y+1/2, -z'
'y+1/2, -x+1/2, -z'
'x+1/2, y+1/2, -z'
'-y+1/2, x+1/2, -z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'x+1/2, -y+1/2, z'
'y+1/2, x+1/2, z'
'-z+1/2, -x+1/2, -y'
'x+1/2, -z+1/2, -y'
'z+1/2, x+1/2, -y'
'-x+1/2, z+1/2, -y'
'-z+1/2, x+1/2, y'
'-x+1/2, -z+1/2, y'
'z+1/2, -x+1/2, y'
'x+1/2, z+1/2, y'
'-y+1/2, -z+1/2, -x'
'z+1/2, y+1/2, x'
'z+1/2, -y+1/2, -x'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb01 Tb 0.000000 0.37097(5) 0.000000 0.0308(6) Uani 1 8 d S T P . .
O1 O 0.000000 0.257(3) 0.000000 0.054(15) Uani 0.25 8 d S TU P . .
O2 O 0.0973(5) 0.3252(5) 0.000000 0.071(3) Uani 1 2 d S T P . .
C1 C 0.2687(9) 0.3139(12) 0.000000 0.135(9) Uani 1 2 d DS TU P . .
H1 H 0.280244 0.355431 0.000000 0.163 Uiso 1 2 calc RS T P . .
C004 C 0.1529(7) 0.3471(7) 0.000000 0.078(6) Uani 1 4 d DS TU P . .
O3 O -0.0579(3) 0.4421(3) -0.0579(3) 0.025(3) Uani 1 6 d S T P . .
C005 C 0.2026(7) 0.2974(7) 0.000000 0.085(7) Uani 1 4 d DS TU 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'
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
Tb01 Tb01 Tb01 60.0 74 33_554 ?
Tb01 Tb01 Tb01 90.000(1) 129 33_554 ?
Tb01 Tb01 Tb01 60.0 129 74 ?
O1 Tb01 Tb01 135.000(1) . 33_554 ?
O1 Tb01 Tb01 135.0 . 129 ?
O1 Tb01 Tb01 135.000(2) . 74 ?
O2 Tb01 Tb01 107.53(18) 114 74 ?
O2 Tb01 Tb01 160.2(3) 20 129 ?
O2 Tb01 Tb01 160.2(3) 114 33_554 ?
O2 Tb01 Tb01 70.2(3) . 74 ?
O2 Tb01 Tb01 160.2(3) 101 74 ?
O2 Tb01 Tb01 107.53(18) 101 129 ?
O2 Tb01 Tb01 107.53(18) . 33_554 ?
O2 Tb01 Tb01 70.2(3) 114 129 ?
O2 Tb01 Tb01 107.53(18) 20 74 ?
O2 Tb01 Tb01 70.2(3) 20 33_554 ?
O2 Tb01 Tb01 107.53(18) 101 33_554 ?
O2 Tb01 Tb01 107.53(18) . 129 ?
O2 Tb01 O1 64.8(3) 20 . ?
O2 Tb01 O1 64.8(3) . . ?
O2 Tb01 O1 64.8(3) 101 . ?
O2 Tb01 O1 64.8(3) 114 . ?
O2 Tb01 O2 79.5(2) 20 101 ?
O2 Tb01 O2 129.6(5) 101 . ?
O2 Tb01 O2 79.5(2) 20 . ?
O2 Tb01 O2 129.6(5) 20 114 ?
O2 Tb01 O2 79.5(2) 101 114 ?
O2 Tb01 O2 79.5(2) 114 . ?
O2 Tb01 O3 78.3(3) 20 74 ?
O2 Tb01 O3 78.3(3) 114 99 ?
O2 Tb01 O3 139.67(16) 101 172 ?
O2 Tb01 O3 139.67(16) 101 74 ?
O2 Tb01 O3 139.67(16) . . ?
O2 Tb01 O3 139.67(16) 114 74 ?
O2 Tb01 O3 78.3(3) . 172 ?
O2 Tb01 O3 78.3(3) . 74 ?
O2 Tb01 O3 139.67(16) 114 . ?
O2 Tb01 O3 139.67(16) . 99 ?
O2 Tb01 O3 139.67(16) 20 172 ?
O2 Tb01 O3 78.3(3) 101 99 ?
O2 Tb01 O3 78.3(3) 114 172 ?
O2 Tb01 O3 139.67(16) 20 99 ?
O2 Tb01 O3 78.3(3) 20 . ?
O2 Tb01 O3 78.3(3) 101 . ?
O3 Tb01 Tb01 32.73(11) 172 129 ?
O3 Tb01 Tb01 85.0(2) 99 33_554 ?
O3 Tb01 Tb01 32.73(11) . 33_554 ?
O3 Tb01 Tb01 32.73(11) 99 129 ?
O3 Tb01 Tb01 85.0(2) 99 74 ?
O3 Tb01 Tb01 85.0(2) 74 129 ?
O3 Tb01 Tb01 85.0(2) 172 33_554 ?
O3 Tb01 Tb01 32.73(11) 74 33_554 ?
O3 Tb01 Tb01 32.73(11) 74 74 ?
O3 Tb01 Tb01 85.0(2) . 129 ?
O3 Tb01 Tb01 32.73(11) 172 74 ?
O3 Tb01 Tb01 85.0(2) . 74 ?
O3 Tb01 O1 131.0(3) 99 . ?
O3 Tb01 O1 131.0(3) . . ?
O3 Tb01 O1 131.0(3) 74 . ?
O3 Tb01 O1 131.0(3) 172 . ?
O3 Tb01 O3 64.5(3) 172 74 ?
O3 Tb01 O3 64.5(3) . 99 ?
O3 Tb01 O3 64.5(3) . 74 ?
O3 Tb01 O3 64.5(3) 172 99 ?
O3 Tb01 O3 98.0(6) 99 74 ?
O3 Tb01 O3 98.0(6) . 172 ?
C004 O2 Tb01 133.2(11) . . ?
C1 C1 H1 119.5 6 . ?
C1 C1 C005 121.0(13) 6 . ?
C005 C1 H1 119.5 . . ?
O2 C004 O2 133(2) 174 . ?
O2 C004 C005 113.4(10) 174 . ?
O2 C004 C005 113.4(10) . . ?
Tb01 O3 Tb01 114.5(2) . 33_554 ?
Tb01 O3 Tb01 114.5(2) . 170_455 ?
Tb01 O3 Tb01 114.5(2) 33_554 170_455 ?
C1 C005 C1 118(3) . 174 ?
C1 C005 C004 121.0(13) 174 . ?
C1 C005 C004 121.0(13) . . ?
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
Tb01 Tb01 3.9337(17) 129 ?
Tb01 Tb01 3.9337(17) 33_554 ?
Tb01 Tb01 3.9337(17) 74 ?
Tb01 O1 2.45(7) . ?
Tb01 O2 2.319(10) 101 ?
Tb01 O2 2.319(10) 114 ?
Tb01 O2 2.319(10) 20 ?
Tb01 O2 2.319(10) . ?
Tb01 O3 2.338(3) 99 ?
Tb01 O3 2.338(3) . ?
Tb01 O3 2.338(3) 74 ?
Tb01 O3 2.338(3) 172 ?
O2 C004 1.288(14) . ?
C1 C1 1.38(5) 6 ?
C1 H1 0.9300 . ?
C1 C005 1.468(17) . ?
C004 C005 1.517(18) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb01 O2 C004 O2 0.0 . . . 174 ?
Tb01 O2 C004 C005 180.0 . . . . ?
O2 C004 C005 C1 180.0 174 . . 174 ?
O2 C004 C005 C1 180.0 . . . . ?
O2 C004 C005 C1 0.0 . . . 174 ?
O2 C004 C005 C1 0.0 174 . . . ?
C1 C1 C005 C1 0.0 6 . . 174 ?
C1 C1 C005 C004 180.0 6 . . . ?
