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_7051361
_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 O2 N4,2(Cl1 O4)'
_chemical_formula_sum            'C10 H22 Cl2 N4 O10'
_chemical_formula_weight         429.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.900(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2700(2)
_cell_length_b                   16.1690(4)
_cell_length_c                   10.8995(2)
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1731.76(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      112(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.022
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7487
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0166(18)
_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   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+1.1613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                4493
_reflns_number_total             4881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005052k.txt
_cod_data_source_block           H2L(ClO4)2
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7051361