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_4313327
_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            'C23 H29 Cl2 Mn N5 O9'
_chemical_formula_weight         645.35
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 127.582(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.053(2)
_cell_length_b                   10.9427(9)
_cell_length_c                   15.5772(16)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.42
_cell_measurement_theta_min      2.22
_cell_volume                     2843.9(5)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3288
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.23
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.8889
_exptl_absorpt_correction_T_min  0.6243
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.64
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.92(5)
_refine_ls_extinction_coef       0.0016(5)
_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   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         3288
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.2539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                2538
_reflns_number_total             3288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020131w_3.cif
_cod_data_source_block           ty-136a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_database_code               4313327