The synthesis of C2-symmetric 1,4,7-triazacyclononane ligands derived from chiral aziridines
Scheuermann, J. Erik W.; Ronketti, Fiona; Motevalli, Majid; Griffiths, D. Vaughan; Watkinson, Michael; New Journal of Chemistry 26 (2002) 1054–; doi:10.1039/b204818c

data_7050957
_publ_section_title
;
 The synthesis of C2-symmetric 1,4,7-triazacyclononane ligands derived
 from chiral aziridines
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1054
_journal_paper_doi               10.1039/b204818c
_journal_volume                  26
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H39 N3 O6 S3'
_chemical_formula_sum            'C33 H45 N3 O6 S3'
_chemical_formula_weight         675.9
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2002-05-10T13:22:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.261(2)
_cell_length_b                   13.805(3)
_cell_length_c                   21.546(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      12.78
_cell_measurement_theta_min      8.234
_cell_measurement_wavelength     0.71073
_cell_volume                     3349.5(11)
_computing_cell_refinement       'CAD4/PC (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4/PC (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.52066E-1
_diffrn_orient_matrix_UB_12      -0.42089E-1
_diffrn_orient_matrix_UB_13      -0.26171E-1
_diffrn_orient_matrix_UB_21      0.20104E-1
_diffrn_orient_matrix_UB_22      0.03986
_diffrn_orient_matrix_UB_23      -0.37288E-1
_diffrn_orient_matrix_UB_31      0.06912
_diffrn_orient_matrix_UB_32      -0.43425E-1
_diffrn_orient_matrix_UB_33      -0.8759E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0047
_diffrn_reflns_av_unetI/netI     0.196
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3415
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.27
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_correction_T_min  0.9481
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.34
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.44
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         3319
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1912
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                1753
_reflns_number_total             3319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204818c.txt
_cod_data_source_block           valmco2
_cod_database_code               7050957
_diffrn_standards_decay_corr_max 1.104
_diffrn_standards_decay_corr_min 0.977