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_7012343
_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         'C40 H80 Cu1 N8 O8'
_chemical_formula_sum            'C10 H18 Cl2 Cu N2 O'
_chemical_formula_weight         316.7
_space_group_IT_number           80
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      80
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2002-06-13T10:38:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.629(4)
_cell_length_b                   26.629(4)
_cell_length_c                   7.506(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.865
_cell_measurement_theta_min      10.208
_cell_measurement_wavelength     0.71073
_cell_volume                     5322.5(18)
_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      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      -0.9924E-2
_diffrn_orient_matrix_UB_12      0.35858E-1
_diffrn_orient_matrix_UB_13      0.17991E-1
_diffrn_orient_matrix_UB_21      -0.36059E-1
_diffrn_orient_matrix_UB_22      -0.9292E-2
_diffrn_orient_matrix_UB_23      -0.17399E-1
_diffrn_orient_matrix_UB_31      -0.3387E-2
_diffrn_orient_matrix_UB_32      -0.6138E-2
_diffrn_orient_matrix_UB_33      0.130861
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.1522
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2688
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.53
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        8
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.024
_exptl_absorpt_correction_T_max  0.589
_exptl_absorpt_correction_T_min  0.12
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         2521
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.2418
_refine_ls_R_factor_gt           0.0923
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+111.9695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1971
_reflns_number_gt                1122
_reflns_number_total             2521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210285d.txt
_cod_data_source_block           4sp73f
_cod_database_code               7012343
_exptl_absorpt_factor_mur        0.405
_exptl_absorpt_correction_t_ave  0.6093
_diffrn_standards_decay_corr_max 1.094
_diffrn_standards_decay_corr_min 0.989