Helical self-assembly of 2-(1,4,7,10-tetraazacyclododecan-1-yl)cyclohexan-1-ol (cycyclen)
de Sousa, Alvaro S.; Sannasy, Denzel; Fernandes, Manuel A.; Marques, Helder M.; Acta Crystallographica Section C 68 (2012) o383–o386; doi:10.1107/S0108270112037195

data_2018598
_publ_section_title
;
 Helical self-assembly of
 2-(1,4,7,10-tetraazacyclododecan-1-yl)cyclohexan-1-ol (cycyclen)
;
_journal_coeditor_code           DT3014
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o383
_journal_page_last               o386
_journal_paper_doi               10.1107/S0108270112037195
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C14 H30 N4 O'
_chemical_formula_moiety         'C14 H30 N4 O'
_chemical_formula_sum            'C14 H30 N4 O'
_chemical_formula_weight         270.42
_chemical_melting_point          418
_chemical_name_common            cycyclen
_chemical_name_systematic
;
2-(1,4,7,10-tetraazacyclododecan-1-yl)cyclohexan-1-ol
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.6137(14)
_cell_length_b                   8.3339(10)
_cell_length_c                   34.350(4)
_cell_measurement_reflns_used    858
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.99
_cell_measurement_theta_min      2.37
_cell_volume                     3038.4(6)
_computing_cell_refinement       'SMART-NT (Bruker, 1998)'
_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            17310
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.218
_refine_ls_extinction_coef       0.0509(19)
_refine_ls_extinction_expression
'Fc^*^ = kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                1813
_reflns_number_total             3127
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dt3014.cif
_cod_data_source_block           I
_cod_database_code               2018598
_cod_database_fobs_code          2018598