Structural Dynamism and Controlled Chemical Blocking/Unblocking of Active Coordination Space of a Soft Porous Crystal
Abhijeet K. Chaudhari; Sanjog S. Nagarkar; Biplab Joarder; Soumya Mukherjee; Sujit K. Ghosh; Inorganic Chemistry 52 (2013) 12784–12789; doi:10.1021/ic402058f

data_4336638
_publ_section_title
;
 Structural Dynamism and Controlled Chemical Blocking/Unblocking of Active
 Coordination Space of a Soft Porous Crystal
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12784
_journal_page_last               12789
_journal_paper_doi               10.1021/ic402058f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C54 H38 Cd3 O20'
_chemical_formula_weight         1344.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 97.359(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.777(2)
_cell_length_b                   10.6187(15)
_cell_length_c                   18.958(3)
_cell_measurement_temperature    200(2)
_cell_volume                     3149.9(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0878
_diffrn_reflns_av_sigmaI/netI    0.1029
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30454
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_T_max  0.9006
_exptl_absorpt_correction_T_min  0.8824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan absorption correction'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       Block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The SQUEEZE routine of the program PLATON was used
in order to eliminate the contribution of disordered solvents molecules,
thereby a final model based only on the ordered part of the crystal structure
was obtained.

The SQUEEZE routine suggested that
a total potential solvent area volume of 974.7 Ang^3^[31.0% of cell volume],
and a void electron population of 235 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.0757 for >2sigma(I) data
R1 = 0.1454, wR2 = 0.2555, GooF = S = 1.000 for all data
( 7909 data and 0 restraint / 385 parameters)
;
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.694
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.694
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0565
_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^)+(0.1389P)^2^+6.4112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                4230
_reflns_number_total             7909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402058f_si_002.cif
_cod_data_source_block           Compound1_ACTN
_cod_original_cell_volume        3149.8(8)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4336638