Thermodynamic, kinetic and solid-state study of divalent metal complexes of 1,4,8,11-tetraazacyclotetradecane (cyclam) bearing two trans (1,8-)methylphosphonic acid pendant arms.
Svobodová, Ivona; Lubal, Premysl; Plutnar, Jan; Havlícková, Jana; Kotek, Jan; Hermann, Petr; Lukes, Ivan; Dalton transactions (Cambridge, England : 2003)  (2006) 5184–5197; doi:10.1039/b603251f

data_7007299
_publ_section_title
;
 Thermodynamic, kinetic and solid-state study of divalent metal
 complexes of 1,4,8,11-tetraazacyclotetradecane (cyclam) bearing two
 trans (1,8-)methylphosphonic acid pendant arms.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5184
_journal_page_last               5197
_journal_paper_doi               10.1039/b603251f
_journal_year                    2006
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety
;
C12 H48 Mn2 N4 O16 P2, C12 H28 N4 O6 P2, (H2 O)21'
;
_chemical_formula_sum            'C24 H118 Mn2 N8 O43 P4'
_chemical_formula_weight         1441.02
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.8084(17)
_cell_angle_beta                 77.3777(17)
_cell_angle_gamma                88.4157(13)
_cell_formula_units_Z            1
_cell_length_a                   9.7361(3)
_cell_length_b                   12.2695(4)
_cell_length_c                   14.0948(4)
_cell_measurement_reflns_used    6889
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1641.51(9)
_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(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13728
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7504
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+2.3729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                5560
_reflns_number_total             7504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603251f.txt
_cod_data_source_block           mndip
_cod_database_code               7007299