Luminescent and magnetic properties of two copper iodide cluster based lanthanide organic frameworks
Shi, Ying; Ren, Xiao-Yang; Gao, Man; Hou, Yin-Ling; Ji, Jia; Wu, Zhi-Lei; Wang, Wen-Min; Inorganica Chimica Acta 506 (2020) 119536–; doi:10.1016/j.ica.2020.119536

data_1564977
_publ_section_title
;
 Luminescent and magnetic properties of two copper iodide cluster based
 lanthanide organic frameworks
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119536
_journal_paper_doi               10.1016/j.ica.2020.119536
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety         '0.13(C168 H64 Cu16 I16 N32 O56 Tb8)'
_chemical_formula_sum            'C21 H8 Cu2 I2 N4 O7 Tb'
_chemical_formula_weight         968.11
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3399(6)
_cell_length_b                   25.3399(6)
_cell_length_c                   9.0750(2)
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.38
_cell_volume                     5827.2(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            37573
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_min         2.384
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.009
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0985 before and 0.0575 after correction.
The Ratio of minimum to maximum transmission is 0.8043.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.207
_exptl_crystal_description       block
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2991
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0346
_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/[\s^2^(Fo^2^)+(0.0494P)^2^+92.1339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2949
_reflns_number_total             2991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-506-119536.cif
_cod_data_source_block           1
_cod_original_cell_volume        5827.2(3)
_cod_database_code               1564977
_shelx_estimated_absorpt_t_max   0.558
_shelx_estimated_absorpt_t_min   0.304
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(3)
 0.03(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 O2_$1-O2_$2
 3.2 with sigma of 0.02
 O1B-O3_$3
 2 with sigma of 0.02
 O1A-C1 \\sim C1-O1B
 with sigma of 0.02
 O1A-Tb1 \\sim Tb1-O1B
 with sigma of 0.02
4. Rigid bond restraints
 C11A, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C10, C11A, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O1B, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1, O1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C11A \\sim C12 \\sim C13: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C7 \\sim N2 \\sim C8: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1B) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11A) = Uanis(C11B)
Uanis(C12) = Uanis(N3)
Uanis(O1A) = Uanis(O1B)
6. Others
 Sof(C11A)=1-FVAR(1)
 Sof(C11B)=FVAR(1)
 Sof(O1B)=1-FVAR(2)
 Sof(O1A)=FVAR(2)
 Fixed Sof: C12(0.5) C13(0.5) N2(0.5) O3(0.5) C7(0.5) N3(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C4(H4)
7.b Fitted hexagon refined as free rotating group:
 C5(N1,C6,C2,C3,C4)
;