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_1564978
_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 Dy8 I16 N32 O56)'
_chemical_formula_sum            'C21 H8 Cu2 Dy I2 N4 O7'
_chemical_formula_weight         971.69
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3670(4)
_cell_length_b                   25.3670(4)
_cell_length_c                   9.0667(2)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.299
_cell_measurement_theta_min      2.385
_cell_volume                     5834.28(18)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            41594
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.378
_diffrn_reflns_theta_min         2.539
_exptl_absorpt_coefficient_mu    6.139
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0808 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.8324.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3584
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 1201 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0230P)^2^+47.6760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2851
_reflns_number_total             2980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-506-119536.cif
_cod_data_source_block           2
_cod_original_cell_volume        5834.3(2)
_cod_database_code               1564978
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C8, N2, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C8 \\sim N2 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
C11A \\sim C12 \\sim C13 \\sim N3 \\sim C11B \\sim C10: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(O3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11B) \\sim Ueq, Uanis(C11A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C11B(0.5) O3(0.5) N3(0.5) N2(0.5) C7(0.5) C11A(0.5) C12(0.5)
 C13(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C4(H4), C5(H5)
;