Thermodynamic and structural aspects of manganese(II) complexes with polyaminopolycarboxylic ligands based upon 1,4,7,10-tetraazacyclododecane (cyclen). Crystal structure of dimeric [MnL]2·2CH3OH containing the new ligand 1,4,7,10-tetraazacyclododecane-1,4-diacetate
Bianchi, Antonio; Calabi, Luisella; Giorgi, Claudia; Losi, Pietro; Mariani, Palma; Palano, Daniela; Paoli, Paola; Rossi, Patrizia; Valtancoli, Barbara; Journal of the Chemical Society, Dalton Transactions  (2001) 917–; doi:10.1039/b009242h

data_7702521
_publ_section_title
;
 Thermodynamic and structural aspects of manganese(II) complexes with
 polyaminopolycarboxylic ligands based upon 1,4,7,10-tetraazacyclododecane
 (cyclen). Crystal structure of dimeric [MnL]2&#x00B7;2CH3OH containing
 the new ligand 1,4,7,10-tetraazacyclododecane-1,4-diacetate
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              917
_journal_paper_doi               10.1039/b009242h
_journal_year                    2001
_chemical_formula_moiety         '(Mn 2+)2, (C12 H22 N4 O4 2-)2, (C H4 O)2'
_chemical_formula_structural     '(Mn2 (C12 H22 N4 O4)2) (C H4 O)2'
_chemical_formula_sum            'C26 H52 Mn2 N8 O10'
_chemical_formula_weight         746.35
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 96.01(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.869(1)
_cell_length_b                   12.965(2)
_cell_length_c                   14.165(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      8.0
_cell_volume                     1619.8(4)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        'Siemens P4'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR97 (Altomare, 1994)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71068
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2958
_diffrn_reflns_theta_max         47
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.46
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   'refdelf (Walker and Stuart, 1983)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.0008(7)
_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_all   1.036
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_obs          0.0778
_refine_ls_shift/esd_max         0.072
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1549P)^2^+4.6252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2174
_refine_ls_wR_factor_obs         0.2104
_reflns_number_observed          2084
_reflns_number_total             2361
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b009242h.txt
_cod_data_source_block           for_[Mn(1,4-DO2A)]2_B72CH3OH
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value '
calc w=1/[\s^2^(Fo^2^)+(0.1549P)^2^+4.6252P] where
P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. A new data item
'_refine_ls_weighting_details' was created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.1549P)^2^+4.6252P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7702521