Formation of columnar hexagonal mesophases near room temperature from functionalised [9]aneNS2 (1,4-dithia-7-azacyclononane)
Blake, Alexander J.; Bruce, Duncan W.; Danks, Jonathan P.; Fallis, Ian A.; Guillon, Daniel; Ross, Steven A.; Richtzenhain, Heiko; Schröder, Martin; Journal of Materials Chemistry 11 (2001) 1011–; doi:10.1039/b006753i

data_7204030
_publ_section_title
;
 Formation of columnar hexagonal mesophases near room temperature from
 functionalised [9]aneNS2 (1,4-dithia-7-azacyclononane)
;
_journal_issue                   4
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1011
_journal_paper_doi               10.1039/b006753i
_journal_volume                  11
_journal_year                    2001
_chemical_formula_moiety         'C13 H17 N O2 S2'
_chemical_formula_sum            'C13 H17 N O2 S2'
_chemical_formula_weight         283.40
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   'at idealised positions, except for O-H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier methods'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.167(2)
_cell_length_b                   13.969(6)
_cell_length_c                   14.443(3)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      12
_cell_volume                     2656.5(13)
_computing_cell_refinement       'Stadi4 (Stoe & Cie, 1995a)'
_computing_data_collection       'Stadi4 (Stoe & Cie, 1995a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1995b)'
_computing_molecular_graphics    'SHELXTL/PC version 5.03 (Sheldrick, 1995)'
_computing_publication_material  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1996)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device
;
Stoe Stadi-4 four-circle diffractometer with Oxford Cryosystems
open-flow crystat
;
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_av_sigmaI/netI    0.038
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3245
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        8.4
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       diamond
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.38
_refine_diff_density_rms         0.10
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876--881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_coef       0.0000(8)
_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_all   1.066
_refine_ls_goodness_of_fit_obs   0.951
_refine_ls_hydrogen_treatment    'riding models'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_restrained_S_obs      0.951
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_obs          0.0574
_refine_ls_shift/esd_max         0.07
_refine_ls_shift/esd_mean        0.01
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+10.339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1870
_refine_ls_wR_factor_obs         0.1545
_reflns_number_observed          2199
_reflns_number_total             2543
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006753i.txt
_cod_data_source_block           PBZNSS
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+10.339P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+10.339P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7204030