Structural, Spectroscopic, and Electrochemical Studies of Binuclear Manganese(II) Complexes of Bis(pentadentate) Ligands Derived from Bis(1,4,7-triazacyclononane) Macrocycles
Suzanne J. Brudenell; Leone Spiccia; Alan M. Bond; Gary D. Fallon; David C. R. Hockless; George Lazarev; Peter J. Mahon; Edward R. T. Tiekink; Inorganic Chemistry 39 (2000) 881–892; doi:10.1021/ic9814470

data_4300005
_publ_section_title
;
Structural, Spectroscopic, and Electrochemical Studies of Binuclear
Manganese(II) Complexes of Bis(pentadentate) Ligands Derived from
Bis(1,4,7-triazacyclononane) Macrocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              881
_journal_page_last               892
_journal_paper_doi               10.1021/ic9814470
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C39 H60 Cl4 Mn2 N10 O11'
_chemical_formula_weight         1096.65
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             1998-09-02
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                90
_cell_angle_beta                 104.328(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.334(2)
_cell_length_b                   19.926(2)
_cell_length_c                   18.799(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      38.6
_cell_measurement_theta_min      28.4
_cell_volume                     4839.4(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device       'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.07108
_diffrn_orient_matrix_UB_12      -0.01617
_diffrn_orient_matrix_UB_13      -0.02472
_diffrn_orient_matrix_UB_21      0.01739
_diffrn_orient_matrix_UB_22      0.00276
_diffrn_orient_matrix_UB_23      -0.04870
_diffrn_orient_matrix_UB_31      0.02524
_diffrn_orient_matrix_UB_32      -0.04743
_diffrn_orient_matrix_UB_33      0.00559
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.06064
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7803
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.09
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        -0.63
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.849
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2280.00
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.615
_refine_ls_goodness_of_fit_obs   2.057
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     595
_refine_ls_number_reflns         3513
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1574
_refine_ls_R_factor_obs          0.0531
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00003|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0712
_refine_ls_wR_factor_obs         0.0605
_reflns_number_observed          3513
_reflns_number_total             7443
_reflns_observed_criterion       >3.00\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00003|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00003|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C39 H60 Cl4 N10 Mn2 O11 '
_cod_database_code               4300005