Chiral cyclopropylamines in the synthesis of new ligands; first asymmetric Alkyl-BIAN compounds.
Hagar, Mohamed; Ragaini, Fabio; Monticelli, Elena; Caselli, Alessandro; Macchi, Piero; Casati, Nicola; Chemical communications (Cambridge, England) 46 (2010) 6153–6155; doi:10.1039/c0cc00977f

data_7113041
_publ_section_title
;
 Chiral cyclopropylamines in the synthesis of new ligands; first
 asymmetric Alkyl-BIAN compounds.
;
_journal_issue                   33
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6153
_journal_page_last               6155
_journal_paper_doi               10.1039/c0cc00977f
_journal_volume                  46
_journal_year                    2010
_chemical_absolute_configuration syn
_chemical_formula_sum            'C17 H22 N4 O7'
_chemical_formula_weight         394.39
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-07-24T16:57:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.181(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.079(4)
_cell_length_b                   12.207(3)
_cell_length_c                   22.502(6)
_cell_measurement_reflns_used    2756
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.4
_cell_measurement_theta_min      2.3
_cell_volume                     3780.2(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17534
_diffrn_reflns_theta_full        22.11
_diffrn_reflns_theta_max         22.11
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         8969
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.107
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+1.7489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1981
_reflns_number_gt                6147
_reflns_number_total             8969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc00977f.txt
_cod_data_source_block           1R,2R,2'R-7
_cod_database_code               7113041