Investigations of the Phase Transitions in Thiourea Inclusion Compounds with Cycloheptane, Cyclooctane, and Cyclooctanone
Thierry Maris; Michael J. Henson; Stephen J. Heyes; Keith Prout; Chem. Mater. 13 (2001) 2483–2492; doi:10.1021/cm991173u

data_4000689
_publ_section_title
;
 Investigations of the Phase Transitions in Thiourea Inclusion Compounds
 with Cycloheptane, Cyclooctane, and Cyclooctanone
;
_journal_name_full               'Chem. Mater.'
_journal_page_first              2483
_journal_page_last               2492
_journal_paper_doi               10.1021/cm991173u
_journal_volume                  13
_journal_year                    2001
_chemical_formula_sum            'C11 H28 N6 S3'
_chemical_formula_weight         340.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             99-02-09
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 113.848(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.4160(6)
_cell_length_b                   30.9180(13)
_cell_length_c                   10.3710(5)
_cell_measurement_reflns_used    12055
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     3641.3(3)
_computing_cell_refinement
;                                                                               
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)                             
;
_computing_data_collection
;                                                                               
DIP2000 software 'Xpress' (MAC Science, 1989)                                   
;
_computing_data_reduction
;                                                                               
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)                             
;
_computing_molecular_graphics
;                                                                               
 CAMERON (Watkin, Prout & Pearce,  1996)                                        
;
_computing_publication_material
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_refinement
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type
;                                                                               
Enraf-nonius DIP2000                                                            
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5397
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.39
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' clear '
_exptl_crystal_density_diffrn    1.24
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             1474.66
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9775
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         3703
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.023733
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
 2.93     1.57     2.14    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0551
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                3703
_reflns_number_total             5397
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           TC8_150K
_cod_original_cell_volume        3641.3
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        ' C22 H56 N12 S6 '
_cod_database_code               4000689