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_4025286
_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         'C58 H59 Cl2 N4 O12'
_chemical_formula_sum            'C58 H59 Cl2 N4 O12'
_chemical_formula_weight         1075.03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-12-19
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 95.320(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.997(5)
_cell_length_b                   18.282(5)
_cell_length_c                   28.996(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     5804(3)
_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 0.970
_diffrn_measured_fraction_theta_max 0.938
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            7620
_diffrn_reflns_theta_full        17.095
_diffrn_reflns_theta_max         22.794
_diffrn_reflns_theta_min         1.797
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.174
_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    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.55
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0190
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         3218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2179
_refine_ls_R_factor_gt           0.1359
_refine_ls_shift/su_max          0.000035
_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: 
 4.15 2.01 2.79 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2289
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1439
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                3218
_reflns_number_total             7376
_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   0.1359
_oxford_refine_ls_scale          0.519(3)
_oxford_reflns_number_all        7332
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'import in P 21/n'
_cod_data_source_file            jo100052r_si_003.cif
_cod_data_source_block           amide
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4025286