A semiconducting microporous framework of Cd6Ag4(SPh)16 clusters interlinked using rigid and conjugated bipyridines
Chao Xu; Niklas Hedin; Hua-Tian Shi; Qian-Feng Zhang; Chem.Commun. 50 (2014) 3710–; doi:10.1039/c3cc49660k

data_7112147
_publ_section_title
;
 A semiconducting microporous framework of Cd6Ag4(SPh)16 clusters
 interlinked using rigid and conjugated bipyridines
;
_journal_name_full               Chem.Commun.
_journal_page_first              3710
_journal_paper_doi               10.1039/c3cc49660k
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C65.63 H63.13 Ag2 Cd3 N3.88 O1.88 S8'
_chemical_formula_weight         1745.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.3203(2)
_cell_length_b                   18.3203(2)
_cell_length_c                   45.4431(11)
_cell_measurement_reflns_used    7157
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.47
_cell_measurement_theta_min      2.22
_cell_volume                     15252.2(4)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Smart APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            44353
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  0.7317
_exptl_absorpt_correction_T_min  0.6145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6920
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;
The unit cell includes disordered solvent
DMF molecules which could not be modeled 
as discrete atomic sites. We employed PLATON/SQUEEZE 
to calculate the diffraction contribution of  
DMF molecules and, thereby, to produce a set of 
solvent-free diraction intensities. The SQUEEZE 
calculations showed the residual electron density amounted 
to 604 e per unit cell, corresponding to nearly 15 molecules 
of DMF.The disordered DMF molecules removed by SQUEEZE
were considered for final calculation of overall 
formula, formula weight, density, F(000), etc.
;
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     286
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.3248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                2891
_reflns_number_total             6539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc49660k2.cif
_cod_data_source_block           i41a
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               7112147