Oligonuclear homo- and mixed-valence manganese complexes based on thiophene- or aryl-carboxylate ligation: Synthesis, characterization and magnetic studies
Reda F.M. Elshaarawy; Yanhua Lan; Christoph Janiak; Inorganica Chimica Acta 401 (2013) 85–94; doi:

data_1517017
_publ_section_title
;
 Oligonuclear homo- and mixed-valence manganese complexes based on
 thiophene- or aryl-carboxylate ligation: Synthesis, characterization and
 magnetic studies
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              85
_journal_page_last               94
_journal_volume                  401
_journal_year                    2013
_chemical_formula_moiety         'C45 H33 Mn3 N3 O13 S6, O'
_chemical_formula_sum            'C45 H33 Mn3 N3 O14 S6'
_chemical_formula_weight         1196.92
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.974(4)
_cell_length_b                   22.931(5)
_cell_length_c                   23.640(5)
_cell_measurement_reflns_used    6914
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.91
_cell_measurement_theta_min      3.00
_cell_volume                     10286(4)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_detector                 RX
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Spider area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Loop
_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  0.1306
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65041
_diffrn_reflns_theta_full        22.91
_diffrn_reflns_theta_max         22.91
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  0.8277
_exptl_absorpt_correction_T_min  0.7604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>ABSCOR</i>; Higashi, 1995)'
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4856
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.308
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.0007(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   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         6914
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1718
_refine_ls_R_factor_gt           0.1016
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1971P)^2^+18.8241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2695
_refine_ls_wR_factor_ref         0.3233
_reflns_number_gt                3778
_reflns_number_total             6914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-401-85-94-2.cif
_cod_data_source_block           pbca
_cod_database_code               1517017