A thiophene-based azacryptand Mannich base: 15,35-dipropyl-2,5,8,22,25,28-hexaoxa-12,18,32,38-tetrathia-15,35-diazapentacyclo[29.5.5.5.0.0]tetraconta-1(37),9(13),10,17(21),19,29(33),30,39-octaene
Gaël Labat; Joan Halfpenny; Acta Crystallographica Section E 62 (2006) o3310–o3312; doi:10.1107/S1600536806026250

data_2209779
_publ_section_title
;A thiophene-based azacryptand Mannich base:
 15,35-dipropyl-2,5,8,22,25,28-hexaoxa-12,18,32,38-tetrathia-15,35-diazapentacyclo[29.5.5.5.0.0]tetraconta-1(37),9(13),10,17(21),19,29(33),30,39-octaene
;
_journal_coeditor_code           CF2037
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3310
_journal_page_last               o3312
_journal_paper_doi               10.1107/S1600536806026250
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C34 H46 N2 O6 S4'
_chemical_formula_sum            'C34 H46 N2 O6 S4'
_chemical_formula_weight         706.97
_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                105.69(2)
_cell_angle_beta                 92.453(18)
_cell_angle_gamma                98.79(2)
_cell_formula_units_Z            1
_cell_length_a                   6.8178(9)
_cell_length_b                   9.4311(18)
_cell_length_c                   13.833(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     842.9(3)
_computing_cell_refinement       'CELL (Stoe & Cie, 2000)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       '\f scans'
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6702
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0468P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                2468
_reflns_number_total             3075
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf2037.cif
_cod_data_source_block           I
_cod_original_cell_volume        842.9(2)
_cod_database_code               2209779
_cod_database_fobs_code          2209779