Coordination properties of cyclam (1,4,8,11-tetraazacyclotetradecane) endowed with two methylphosphonic acid pendant arms in the 1,4-positions
Havlíčková, Jana; Medová, Hana; Vitha, Tomáš; Kotek, Jan; Císařová, Ivana; Hermann, Petr; Dalton Transactions  (2008) 5378–5386; doi:10.1039/b803235a

data_7004149
_publ_section_title
;
 Coordination properties of cyclam (1,4,8,11-tetraazacyclotetradecane)
 endowed with two methylphosphonic acid pendant arms in the
 1,4-positions
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              5378
_journal_page_last               5386
_journal_paper_doi               10.1039/b803235a
_journal_year                    2008
_chemical_formula_moiety         '3(C12 H28 N4 Ni O6 P2), 5(H2 O)'
_chemical_formula_sum            'C36 H94 N12 Ni3 O23 P6'
_chemical_formula_weight         1425.18
_chemical_name_systematic
;
?
;
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.26620(10)
_cell_length_b                   15.26620(10)
_cell_length_c                   43.2280(4)
_cell_measurement_reflns_used    6775
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     8724.84(11)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            13307
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale violet'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         13307
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          1.315
_refine_ls_shift/su_mean         0.216
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+21.4274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                9407
_reflns_number_total             13307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b803235a.txt
_cod_data_source_block           ni
_cod_database_code               7004149