cis-Diprotected cyclams and cyclens: a new route to symmetrically or asymmetrically 1,4-disubstituted tetraazamacrocycles and to asymmetrically tetrasubstituted derivatives
Bellouard, Frédéric; Chuburu, Françoise; Kervarec, Nelly; Toupet, Loïc; Triki, Smaïl; Le Mest, Yves; Handel, Henri; Journal of the Chemical Society, Perkin Transactions 1  (1999) 3499–; doi:10.1039/a905701c

data_7213158
_publ_section_title
;
 cis-Diprotected cyclams and cyclens: a new route to symmetrically or
 asymmetrically 1,4-disubstituted tetraazamacrocycles and to
 asymmetrically tetrasubstituted derivatives
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              3499
_journal_paper_doi               10.1039/a905701c
_journal_year                    1999
_chemical_formula_moiety         C24H36N4O8Cl2Ni
_chemical_formula_sum            'C24 H36 Cl2 N4 Ni O8'
_chemical_formula_weight         638.19
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 91.55(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   9.785(1)
_cell_length_b                   27.604(3)
_cell_length_c                   10.306(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      10.0
_cell_volume                     2782.7(5)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1994)
_computing_data_collection       CAD4_(Enraf-Nonius,_1994)
_computing_data_reduction        process_MolEN_(Fair,_1990)
_computing_publication_material  BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990)
_computing_structure_refinement  LSFM_MolEN_(Fair,_1990)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      294
_diffrn_measurement_device_type  Enraf_Nonius_CAD4
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.103
_diffrn_reflns_av_sigmaI/netI    0.667
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5312
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  25
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.52
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.266
_refine_ls_abs_structure_details ' ? '
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   8.999
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    refxyz_U=1.3_x_bonding_atom
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     352
_refine_ls_number_reflns         1719
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.246
_refine_ls_R_factor_gt           0.054
_refine_ls_shift/esd_mean        0.031
_refine_ls_shift/su_max          0.526
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.396
_refine_ls_wR_factor_ref         0.061
_reflns_number_gt                1719
_reflns_number_total             4761
_reflns_threshold_expression     >1.5\s(I)
_cod_data_source_file            905701csup1.cif
_cod_data_source_block           nicyclamdibenz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) + 0.0064
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w =
4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2782.6(9)
_cod_original_formula_sum        C24H36N4O8Cl2Ni
_cod_database_code               7213158