Synthesis, structure and luminescent properties of two Cd(II)/M(I) (M = K, Rb) interpenetrated heterometallic frameworks based on giant double-walled cages
Xu, Xiao-Wu; Tian, Chong-Bin; Du, Shaowu; CrystEngComm  (2017) –; doi:10.1039/C7CE00803A

data_7228543
_publ_section_title
;
 Synthesis, structure and luminescent properties of two Cd(II)/M(I) (M =
 K, Rb) interpenetrated heterometallic frameworks based on giant
 double-walled cages
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00803A
_journal_year                    2017
_chemical_formula_sum            'C68 H79.5 Cd3 K6 N16 O39.75'
_chemical_formula_weight         2328.77
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_Hall           'I 4 2 3'
_space_group_name_H-M_alt        'I 4 3 2'
_symmetry_space_group_name_Hall  'I 4 2 3'
_symmetry_space_group_name_H-M   'I 4 3 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-01 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.9730(10)
_cell_length_b                   27.9730(10)
_cell_length_c                   27.9730(10)
_cell_measurement_reflns_used    30024
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.0587
_cell_volume                     21888.6(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            94403
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         3.714
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sphere(Rigaku Crystalclear)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       Cubic
_exptl_crystal_F_000             9404
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;                          
 The unit cell contains 32 DMF molecules and 16 CH3OH molecules which have been
 treated as a diffuse contribution to the overall scattering without specific atom
 positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4166
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0593P)^2^+33.2729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4116
_reflns_number_total             4166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00803a2.cif
_cod_data_source_block           A
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        21889(2)
_cod_original_formula_sum        'C68 H79.50 Cd3 K6 N16 O39.75'
_cod_database_code               7228543
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              10685