Structure, modelling and dynamic behaviour of aza- and azaoxamacrocyclic ligands derived from (R,R)-1,2-diaminocyclohexaneElectronic supplementary information (ESI) available: different views of compounds 6, 6a and 6b. See http://www.rsc.org/suppdata/ob/b3/b306963j/
Pulacchini, Sonia; Nasser, Rima; Sibbons, Kevin F.; Motevalli, Majid; Hawkes, Geoffrey E.; Kroemer, Romano T.; Bento, Edson S.; Watkinson, Michael; Organic & Biomolecular Chemistry 1 (2003) 4058–; doi:10.1039/b306963j

data_7151516
_publ_section_title
;
 Structure, modelling and dynamic behaviour of aza- and
 azaoxamacrocyclic ligands derived from
 (R,R)-1,2-diaminocyclohexaneElectronic supplementary information (ESI)
 available: different views of compounds 6, 6a and 6b. See
 http://www.rsc.org/suppdata/ob/b3/b306963j/
;
_journal_issue                   22
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              4058
_journal_paper_doi               10.1039/b306963j
_journal_volume                  1
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C48 H64 N2 O4 S2'
_chemical_formula_structural     'C48 H64 N2 O4 S2'
_chemical_formula_sum            'C24 H33 N2 O5.5 S2'
_chemical_formula_weight         501.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        '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/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-04-04T15:03:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.09(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.905(8)
_cell_length_b                   17.292(3)
_cell_length_c                   9.515(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      11.41
_cell_measurement_theta_min      9.16
_cell_measurement_wavelength     0.71073
_cell_volume                     2448.8(15)
_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)'
_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      -0.18396E-1
_diffrn_orient_matrix_UB_12      -0.38233E-1
_diffrn_orient_matrix_UB_13      -0.74967E-1
_diffrn_orient_matrix_UB_21      -0.63457E-1
_diffrn_orient_matrix_UB_22      0.2717E-2
_diffrn_orient_matrix_UB_23      0.28821E-1
_diffrn_orient_matrix_UB_31      -0.12216E-1
_diffrn_orient_matrix_UB_32      0.43302E-1
_diffrn_orient_matrix_UB_33      -0.68018E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            4888
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.81
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        -4
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.9502
_exptl_absorpt_correction_T_min  0.8819
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   3
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(10)
_refine_ls_extinction_coef       0.0014(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+1.6805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                3284
_reflns_number_total             4461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306963j.txt
_cod_data_source_block           spnno1
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-08-02

The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'PSI SCAN' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     '-P 2yb'
_cod_original_sg_symbol_H-M      P21
_cod_original_formula_sum        'C24 H33 N2 O5.50 S2'
_cod_database_code               7151516
_diffrn_standards_decay_corr_max 1.054
_diffrn_standards_decay_corr_min 0.906