Synthesis of C2-symmetric aza- and azaoxa-macrocyclic ligands derived from (1R,2R)-1,2-diaminocyclohexane and their applications in catalysisBased on the presentation given at Dalton Discussion No. 5, 10?12th April 2003, Noordwijkerhout, The Netherlands.
Pulacchini, Sonia; Sibbons, Kevin F.; Shastri, Kirtida; Motevalli, Majid; Watkinson, Michael; Wan, Hayley; Whiting, Andrew; Lightfoot, Andrew P.; Dalton Transactions  (2003) 2043–; doi:10.1039/b210285d

data_7012344
_publ_section_title
;
 Synthesis of C2-symmetric aza- and azaoxa-macrocyclic ligands derived
 from (1R,2R)-1,2-diaminocyclohexane and their applications in
 catalysisBased on the presentation given at Dalton Discussion No. 5,
 10?12th April 2003, Noordwijkerhout, The Netherlands.
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              2043
_journal_paper_doi               10.1039/b210285d
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H27 N3 O3 S1'
_chemical_formula_sum            'C18 H27 N3 O3 S'
_chemical_formula_weight         365.49
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      76
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_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      2.2
_audit_creation_date             2002-10-15T13:20:25-00:00
_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                   11.164(2)
_cell_length_b                   11.164(2)
_cell_length_c                   14.910(3)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      11.713
_cell_measurement_theta_min      9.2875
_cell_measurement_wavelength     0.71073
_cell_volume                     1858.3(6)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'PLATON (Spek, 1998)'
_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      180(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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      0.078961
_diffrn_orient_matrix_UB_12      -0.041925
_diffrn_orient_matrix_UB_13      0.003378
_diffrn_orient_matrix_UB_21      -0.041236
_diffrn_orient_matrix_UB_22      -0.074495
_diffrn_orient_matrix_UB_23      0.020307
_diffrn_orient_matrix_UB_31      -0.008817
_diffrn_orient_matrix_UB_32      -0.025787
_diffrn_orient_matrix_UB_33      -0.063888
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.2394
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1553
_diffrn_reflns_theta_full        23.05
_diffrn_reflns_theta_max         23.05
_diffrn_reflns_theta_min         1.82
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_correction_T_min  0.3585
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         1351
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.2105
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1818
_reflns_number_gt                682
_reflns_number_total             1351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210285d.txt
_cod_data_source_block           isp78
_cod_database_code               7012344
_exptl_absorpt_factor_mur        0.02
_diffrn_standards_decay_corr_max 1.035
_diffrn_standards_decay_corr_min 0.988