Synthesis, characterization and X-ray crystal structures of cyclam derivatives. Part IV. 1,4,8,11-Tetraazacyclotetradecane-5,12-dione and its diprotonated forms
Laurent Frémond; Enrique Espinosa; Michel Meyer; Franck Denat; Roger Guilard; Volker Huch; Michael Veith; New J. Chem. 24 (2000) 959–966; doi:10.1039/b005052k

data_7051360
_publ_section_title
;
 Synthesis, characterization and X-ray crystal structures of cyclam
 derivatives. Part IV. 1,4,8,11-Tetraazacyclotetradecane-5,12-dione and
 its diprotonated forms
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              959
_journal_page_last               966
_journal_paper_doi               10.1039/b005052k
_journal_volume                  24
_journal_year                    2000
_chemical_formula_moiety         'C10 H22 N4 O2,Br2'
_chemical_formula_sum            'C10 H22 Br2 N4 O2'
_chemical_formula_weight         390.14
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.126(3)
_cell_angle_beta                 104.189(3)
_cell_angle_gamma                97.989(3)
_cell_formula_units_Z            1
_cell_length_a                   5.2851(2)
_cell_length_b                   8.0718(4)
_cell_length_c                   9.5424(5)
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     362.03(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2142
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    5.600
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             196
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.029(4)
_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   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.4758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                1550
_reflns_number_total             1619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005052k.txt
_cod_data_source_block           H2LBr2
_cod_database_code               7051360