A Stepwise Mechanism for the Mechanochemical Synthesis of Halogen-Bonded Cocrystal Architectures
Dominik Cinčić; Tomislav Friščić; William Jones; Journal of the American Chemical Society 130 (2008) 7524–7525; doi:10.1021/ja801164v

data_4107900
_publ_section_title
;
 A Stepwise Mechanism for the Mechanochemical Synthesis of Halogen-Bonded
 Cocrystal Architectures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7524
_journal_page_last               7525
_journal_paper_doi               10.1021/ja801164v
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         '2(C4 H9 N1 S), (C6 F4 I2)'
_chemical_formula_sum            'C14 H18 F4 I2 N2 S2'
_chemical_formula_weight         608.22
_chemical_name_common            (1,4-tfib).(tmo)2
_chemical_name_systematic
;
 1,4-diiodotetrafluorobenzene-1,4-thiomorpholine 1/2
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.2090(10)
_cell_angle_beta                 96.1850(10)
_cell_angle_gamma                99.3710(10)
_cell_formula_units_Z            1
_cell_length_a                   5.23140(10)
_cell_length_b                   6.10850(10)
_cell_length_c                   15.3239(3)
_cell_measurement_reflns_used    6158
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      1.00
_cell_volume                     470.778(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9236
_diffrn_reflns_theta_full        34.98
_diffrn_reflns_theta_max         34.98
_diffrn_reflns_theta_min         3.95
_exptl_absorpt_coefficient_mu    3.599
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.145
_exptl_crystal_description       prism
_exptl_crystal_F_000             290
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.604
_refine_diff_density_min         -2.713
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.081(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         4050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0521P)^2^+0.2973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                3918
_reflns_number_total             4050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801164v-file002.cif
_cod_data_source_block           (1,4-tfib).(tmo)2
_cod_database_code               4107900