A novel (3,3,6)-connected luminescent metal-organic framework for sensing of nitroaromatic explosives.
Sun, Libo; Xing, Hongzhu; Xu, Jin; Liang, Zhiqiang; Yu, Jihong; Xu, Ruren; Dalton transactions (Cambridge, England : 2003) 42 (2013) 5508–5513; doi:10.1039/c3dt32851a

data_7022688
_publ_section_title
;
 A novel (3,3,6)-connected luminescent metal-organic framework for sensing
 of nitroaromatic explosives.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5508
_journal_page_last               5513
_journal_paper_doi               10.1039/c3dt32851a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C42.5 H14 Cd3 N3 O15'
_chemical_formula_weight         1143.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.6200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.7480(18)
_cell_length_b                   18.5200(9)
_cell_length_c                   24.4110(13)
_cell_measurement_temperature    296(2)
_cell_volume                     14186.7(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            63139
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.563
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.315
_platon_squeeze_details
;
The remaining solvent molecules were disordered and assigned as 8 DMF molecules,
8 ethanol molecules and 16 water molecules per unit cell, which were determined by TGA,
elemental analysis and SQUEEZE results. The contributions of these disordered solvents to
the scattering values have been removed by using the PLATON SQUEEZE program. We can see from
the SQUEEZE that there are about 853e in the unit cell, as about 107e per asymmetric unit, which
include 21e of H of coordinated DMF molecules and 86e of free solvent. From the calculation and
related information (The CHN and TGA), the asymmetric unit should include one DMF, one C2H5OH and two H2O (40e+26e+10e*2=86e).
Anal. Cald. for C47.5H52Cd3N4O19: C, 43.21; H, 3.97; N, 4.24; found: C, 42.97; H, 4.23; N, 4.34.
Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         15805
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.126
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                9412
_reflns_number_total             15805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32851a.txt
_cod_data_source_block           cc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        14186.7(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C42.50 H14 Cd3 N3 O15'
_cod_database_code               7022688