A New Class of C3-Symmetrical Hemicryptophane Hosts: Triamide- and Tren-hemicryptophanes
Pascal Dimitrov Raytchev; Olivier Perraud; Christophe Aronica; Alexandre Martinez; Jean-Pierre Dutasta; Journal of Organic Chemistry 75 (2010) 2099–2102; doi:10.1021/jo100052r

data_4025285
_publ_contact_author_address
; Ecole Normale Sup\'erieure de Lyon,
Laboratoire de Chimie,
46 all\'ee d'Italie
69364 Lyon Cedex 07
France
;
_publ_contact_author_email       christophe.aronica@ens-lyon.fr
_publ_contact_author_fax         +0033472728860
_publ_contact_author_name        'Christophe Aronica'
_publ_contact_author_phone       +0033472728864
_publ_section_title
;
 A New Class of C3-Symmetrical Hemicryptophane Hosts: Triamide- and
 Tren-hemicryptophanes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2099
_journal_page_last               2102
_journal_paper_doi               10.1021/jo100052r
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C185.99 H230.96 N12.00 O27'
_chemical_formula_sum            'C185.99 H230.96 N12 O27'
_chemical_formula_weight         3066.72
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-04-07
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.610(19)
_cell_length_b                   16.610(8)
_cell_length_c                   37.237(11)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     8897(11)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       Unknown
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            7275
_diffrn_reflns_theta_full        21.274
_diffrn_reflns_theta_max         24.175
_diffrn_reflns_theta_min         1.521
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3293.730
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1275
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         1828
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1882
_refine_ls_R_factor_gt           0.1390
_refine_ls_shift/su_max          0.000280
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 14.1 9.34 8.32 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2369
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1706
_reflns_limit_h_max              9
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              42
_reflns_limit_l_min              0
_reflns_number_gt                1469
_reflns_number_total             2998
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1491
_oxford_refine_ls_scale          1.667(14)
_oxford_reflns_number_all        2973
_oxford_reflns_threshold_expression_ref I>1.0\s(I)
_oxford_structure_analysis_title 'lala in R -3'
_cod_data_source_file            jo100052r_si_002.cif
_cod_data_source_block           amine
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        8897(13)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C185.99 H230.96 N12.00 O27'
_cod_database_code               4025285