Topochemical conversion of a dense metal‒organic framework from a crystalline insulator to an amorphous semiconductor
Tominaka, S.; Hamoudi, H.; Suga, T.; Bennett, T. D.; Cairns, A. B.; Cheetham, A. K.; Chem. Sci. 6 (2015) 1465–; doi:10.1039/C4SC03295K

data_1518352
_publ_section_title
;
 Topochemical conversion of a dense metal--organic framework from a
 crystalline insulator to an amorphous semiconductor
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1465
_journal_paper_doi               10.1039/C4SC03295K
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         '0.25(C12 H12 Cl4 Cu4 N12 S12)'
_chemical_formula_sum            'C3 H3 Cl Cu N3 S3'
_chemical_formula_weight         276.25
_chemical_name_systematic        'Cu(I)Cl trithiocyanurate'
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_audit_update_record
;
2014-08-10 deposited with the CCDC.
2014-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.70071(13)
_cell_length_b                   11.70071(13)
_cell_length_c                   11.70071(13)
_cell_measurement_reflns_used    1386
_cell_measurement_temperature    120.05(10)
_cell_measurement_theta_max      67.5890
_cell_measurement_theta_min      6.5320
_cell_volume                     1601.90(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.05(10)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0183430000
_diffrn_orient_matrix_UB_12      -0.1163857000
_diffrn_orient_matrix_UB_13      0.0581751000
_diffrn_orient_matrix_UB_21      -0.0477732000
_diffrn_orient_matrix_UB_22      0.0609971000
_diffrn_orient_matrix_UB_23      0.1064942000
_diffrn_orient_matrix_UB_31      -0.1215467000
_diffrn_orient_matrix_UB_32      -0.0065601000
_diffrn_orient_matrix_UB_33      -0.0507897000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1999
_diffrn_reflns_theta_full        67.63
_diffrn_reflns_theta_max         67.63
_diffrn_reflns_theta_min         6.55
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.689
_exptl_absorpt_correction_T_max  0.214
_exptl_absorpt_correction_T_min  0.099
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             1088
_exptl_crystal_preparation
'CuCl and trithiocyanuric acid were heated in acetonitrile at 90C.'
_exptl_crystal_recrystallization_method
'Solvothermal reaction of CuCl and trithiocyanuric acid in acetonitrile'
_exptl_crystal_size_max          0.2928
_exptl_crystal_size_mid          0.2532
_exptl_crystal_size_min          0.2028
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.9651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                462
_reflns_number_total             484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc03295k1.cif
_cod_data_source_block           2-157_cu_120k_abs_2
_cod_depositor_comments
'Adding full bibliography for 1518352--1518354.cif.'
_cod_database_code               1518352
_chemical_oxdiff_formula         'Cu Cl C3 N3 S3 H3'
_reflns_odcompleteness_completeness 94.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'