Dioxo-Bridged Dinuclear Manganese(III) and -(IV) Complexes of Pyridyl Donor Tripod Ligands: Combined Effects of Steric Substitution and Chelate Ring Size Variations on Structural, Spectroscopic, and Electrochemical Properties
Yilma Gultneh; Teshome B. Yisgedu; Yohannes T. Tesema; Ray J. Butcher; Inorganic Chemistry 42 (2003) 1857–1867; doi:10.1021/ic020131w

data_4313325
_publ_section_title
;
 Dioxo-Bridged Dinuclear Manganese(III) and -(IV) Complexes of Pyridyl
 Donor Tripod Ligands: Combined Effects of Steric Substitution and Chelate
 Ring Size Variations on Structural, Spectroscopic, and Electrochemical
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1857
_journal_page_last               1867
_journal_paper_doi               10.1021/ic020131w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C42 H48 Cl2 Mn2 N8 O10'
_chemical_formula_weight         1005.66
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.628(6)
_cell_angle_beta                 80.426(7)
_cell_angle_gamma                86.505(7)
_cell_formula_units_Z            1
_cell_length_a                   9.0081(7)
_cell_length_b                   11.5356(10)
_cell_length_c                   11.8101(10)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.19
_cell_measurement_theta_min      1.96
_cell_volume                     1102.26(17)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_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  0.0145
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5236
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.10
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.8673
_exptl_absorpt_correction_T_min  0.5658
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.99
_exptl_crystal_size_min          0.76
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.034(3)
_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_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.5104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                4551
_reflns_number_total             4928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020131w_1.cif
_cod_data_source_block           ty189c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

2021-04-13
Formula fixed to be consistent with given Z value
                 miguel
;
_cod_original_cell_volume        1102.26(16)
_cod_original_formula_sum        'C21 H24 Cl Mn N4 O5'
_cod_original_formula_weight     502.83
_cod_database_code               4313325