The in, out Asymmetric Pseudo-Triple Helical Form of a D_3h_ Diaza-Macropentacycle
Clément Bonnot; Jean-Claude Chambron; Enrique Espinosa; Roland Graff; Journal of Organic Chemistry 73 (2008) 868–881; doi:10.1021/jo701984z

data_4023226
_publ_section_title
;
 The in, out Asymmetric Pseudo-Triple Helical Form of a D_3h_
 Diaza-Macropentacycle
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              868
_journal_page_last               881
_journal_paper_doi               10.1021/jo701984z
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C129 H162 N8 O12 S12, 8.5(C2 H3 N)'
_chemical_formula_sum            'C146 H187.5 N16.5 O12 S12'
_chemical_formula_weight         2750.34
_chemical_name_systematic
;
 ?
;
_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                103.545(1)
_cell_angle_beta                 95.190(1)
_cell_angle_gamma                100.435(1)
_cell_formula_units_Z            2
_cell_length_a                   15.578(2)
_cell_length_b                   20.630(3)
_cell_length_c                   25.818(4)
_cell_measurement_reflns_used    49348
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      1.76
_cell_volume                     7856(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49348
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2934
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2198
_refine_ls_number_reflns         27410
_refine_ls_number_restraints     895
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0996
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+35.8376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2179
_reflns_number_gt                21913
_reflns_number_total             27410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo701984z-File005.cif
_cod_data_source_block           cbo006
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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 
;
_cod_original_formula_sum        'C146 H187.50 N16.50 O12 S12'
_cod_database_code               4023226