Structure and conformational analysis of a bidentate pro-ligand, C~21~H~34~N~2~S~2~, from powder synchrotron diffraction data and solid-state DFTB calculations
Ávila, Edward E.; Mora, Asiloé J.; Delgado, Gerzon E.; Contreras, Ricardo R.; Rincón, Luis; Fitch, Andrew N.; Brunelli, Michela; Acta Crystallographica Section B 65 (2009) 639–646; doi:10.1107/S0108768109027244

data_2104475
_publ_section_title
;
 Structure and conformational analysis of a bidentate pro-ligand,
 C~21~H~34~N~2~S~2~, from powder synchrotron diffraction data and
 solid-state DFTB calculations
;
_journal_coeditor_code           ZB5006
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              639
_journal_page_last               646
_journal_paper_doi               10.1107/S0108768109027244
_journal_volume                  65
_journal_year                    2009
_chemical_formula_analytical     'C21 H34 N2 S2'
_chemical_formula_moiety         'C21 H34 N2 S2'
_chemical_formula_sum            'C21 H34 N2 S2'
_chemical_formula_weight         378.64
_chemical_name_systematic
;
ethyl 1',2',3',4',4a',5',6',7'-octahydrodispiro[cyclohexane-1,2'-
quinazoline-4',1''-cyclohexane]-8'-carbodithioate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'from EXP file using GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 99.9602(8)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   21.7356(4)
_cell_length_b                   10.0565(2)
_cell_length_c                   9.45108(18)
_cell_measurement_temperature    298.0(10)
_cell_volume                     2034.72(7)
_computing_molecular_graphics
'PLATON (Spek, 2003) and DIAMOND 2.1e (Brandenburg, 2001)'
_computing_publication_material
;GSAS2CIF (Toby et al., 2003), PLATON (Spek, 2003), and publCIF (Westrip,
 2009)
;
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type
'High Resolution Diffractometer ID31, ESRF, Grenoble, France.'
_diffrn_radiation_monochromator  'Double crystal Si 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80098
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_process_details   none
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_F_000             824
_pd_block_id
2009-05-20T11:14|ZB5006_13|Edward_E.\'Avila_S.|ID31,_ESRF,_Grenoble-France
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  yellow
_pd_char_particle_morphology     'thin powder'
_pd_instr_location
'High Resolution Diffractometer ID31, ESRF, Grenoble, France.'
_pd_meas_number_of_points        15665
_pd_meas_scan_method             step
_pd_phase_name                   'from C:/gsas/MyWork/ZB5006_13/geom01e_01.cif'
_pd_prep_temperature             298.0(10)
_pd_proc_info_datetime           2009-05-20T11:14:14
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 20 terms.
 Shifted Chebyshev function of 1st kind
      1:    1003.18     2:   -242.455     3:    44.5847     4:    55.6979
      5:   -29.4706     6:   -81.1134     7:    127.180     8:   -98.3496
      9:    20.8256    10:    37.3447    11:   -40.7733    12:    13.3524
     13:    13.5172    14:   -16.2420    15:    32.6866    16:    8.33642
     17:   -35.1107    18:    7.23691    19:    5.42771    20:    5.20341
;
_pd_proc_ls_peak_cutoff          0.00150
_pd_proc_ls_pref_orient_corr     'Spherical Harmonic'
_pd_proc_ls_profile_function
;CW Profile function number 4 with 21 terms Pseudovoigt profile coefficients
 as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl.
 Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P.
 Jephcoat (1994). J. Appl. Cryst.,27,892-900. Microstrain broadening by P.W.
 Stephens, (1999). J. Appl. Cryst.,32,281-289. Peak tails are ignored where
 the intensity is below 0.0015 times the peak Aniso. broadening axis 0.0 0.0
 1.0
;
_pd_proc_ls_prof_R_factor        0.0439
_pd_proc_ls_prof_wR_expected     0.0237
_pd_proc_ls_prof_wR_factor       0.0540
_pd_proc_number_of_points        15665
_pd_proc_wavelength              0.80098
_pd_spec_mounting                'borosilicate glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              40
_pd_spec_size_equat              10
_pd_spec_size_thick              10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.30
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    1
_refine_ls_number_parameters     127
_refine_ls_number_restraints     186
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Inet
_reflns_number_total             1374
_cod_data_source_file            zb5006.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               2104475
_cod_database_fobs_code          2104475