Dynamic Metal-Organic Framework with Anion-Triggered Luminescence Modulation Behavior.
Karmakar, Avishek; Manna, Biplab; Desai, Aamod V.; Joarder, Biplab; Ghosh, Sujit K.; Inorganic chemistry  (2014) 141118130516009–; doi:10.1021/ic501477u

data_4341731
_publ_section_title
;
 Dynamic Metal-Organic Framework with Anion-Triggered Luminescence
 Modulation Behavior.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141118130516009
_journal_paper_doi               10.1021/ic501477u
_journal_year                    2014
_chemical_formula_moiety         'C16 H22 Cl2 N10 O10 Zn'
_chemical_formula_sum            'C16 H22 Cl2 N10 O10 Zn'
_chemical_formula_weight         650.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.597(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.740(4)
_cell_length_b                   12.600(2)
_cell_length_c                   15.198(3)
_cell_measurement_reflns_used    7266
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.23
_cell_volume                     3456.5(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14263
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.225
_diffrn_reflns_theta_min         1.971
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.9058
_exptl_absorpt_correction_T_min  0.8978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan absorption correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_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 1223.4Ang^3^[35.4% of cell volume],

and a void electron population of 364 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.

[R values before SQUEEZE]

R1 = 0.1270, wR2 = 0.4146 for >2sigma(I) data

R1 = 0.1343, wR2 = 0.4271, GooF = S = 2.119 for all data

( 3470 data and 0 restraint / 178 parameters)

;
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+25.4494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3078
_reflns_number_total             3470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501477u_si_003.cif
_cod_data_source_block           Compound1ClO4
_cod_original_cell_volume        3456.5(12)
_cod_database_code               4341731
_shelx_estimated_absorpt_t_min   0.898
_shelx_estimated_absorpt_t_max   0.906
_shelxl_version_number           2013-3
_shelx_res_checksum              93808
_shelx_hkl_checksum              50939