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_4023224
_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         'C44.75 H56.75 Cl0.50 N2.75 O6.50 S4'
_chemical_formula_sum            'C44.75 H56.75 Cl0.5 N2.75 O6.5 S4'
_chemical_formula_weight         883.14
_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                90.004(1)
_cell_angle_beta                 95.224(1)
_cell_angle_gamma                108.017(1)
_cell_formula_units_Z            2
_cell_length_a                   9.6679(2)
_cell_length_b                   12.5864(2)
_cell_length_c                   19.7850(5)
_cell_measurement_reflns_used    16611
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.63
_cell_volume                     2278.94(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0924
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16611
_diffrn_reflns_theta_full        27.36
_diffrn_reflns_theta_max         27.36
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         10287
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                6216
_reflns_number_total             10287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo701984z-File003.cif
_cod_data_source_block           cbo001
_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        'C44.75 H56.75 Cl0.50 N2.75 O6.50 S4'
_cod_database_code               4023224