Bis(dimethylformamide)pentakis(μ-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetrakis(1-methylimidazole)di-μ-propionato-pentamanganese(III)manganese(II)‒dimethylformamide‒methanol (1/0.24/1.36)
Lutter, Jacob C.; Kampf, Jeff W.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 69 (2013) m483–m484; doi:10.1107/S1600536813021314

data_2238514
_publ_section_title
;
 Bis(dimethylformamide)pentakis(\m-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetrakis(1-methylimidazole)di-\m-propionato-pentamanganese(III)manganese(II)--dimethylformamide--methanol
 (1/0.24/1.36)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m483
_journal_page_last               m484
_journal_paper_doi               10.1107/S1600536813021314
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
;[Mn6 (C7 H4 N O3)5 (C3 H5 O2)2 (C4 H6 N2)4.17 (C3 H7 N O)1.83], 0.24C3 H7 N O
 , 1.36 CH4 O
;
_chemical_formula_moiety
'C63.174 H67.826 Mn6 N15.174 O20.826, 0.243(C3 H7 N O), 1.361(C H4 O)'
_chemical_formula_sum            'C65.264 H74.971 Mn6 N15.417 O22.43'
_chemical_formula_weight         1763.91
_chemical_name_systematic
'Bis(dimethylformamide)pentakis(\m-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetrakis(1-methylimidazole)di-\m-propionato-pentamanganese(III)manganese(II)--dimethylformamide--methanol (1/0.24/1.36)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2012
_cell_angle_alpha                97.909(7)
_cell_angle_beta                 105.209(7)
_cell_angle_gamma                99.034(7)
_cell_formula_units_Z            2
_cell_length_a                   12.6138(2)
_cell_length_b                   14.8745(3)
_cell_length_c                   20.7862(15)
_cell_measurement_reflns_used    45007
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.20
_cell_volume                     3650.7(3)
_computing_cell_refinement
'<i>CrystalClear-SM Expert</i> (Rigaku, 2011)'
_computing_data_collection
'<i>CrystalClear-SM Expert</i> (Rigaku, 2011)'
_computing_data_reduction
'<i>CrystalClear-SM Expert</i> (Rigaku, 2011)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2008) and
<i>SHELXLE</i> (H\"ubschle <i>et al.</i>, 2011)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            106589
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         2.242
_exptl_absorpt_coefficient_mu    8.930
_exptl_absorpt_correction_T_max  0.233
_exptl_absorpt_correction_T_min  0.179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>REQAB</i>; Jacobson, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       needle
_exptl_crystal_F_000             1807.8
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.583
_refine_ls_extinction_coef       0.00166(14)
_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   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1153
_refine_ls_number_reflns         13145
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1023P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1638
_reflns_number_gt                10454
_reflns_number_total             13145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jj2172.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C65.264 H74.971 Mn6 N15.417 O22.430'
_cod_database_code               2238514
_cod_database_fobs_code          2238514
_shelx_estimated_absorpt_t_min   0.574
_shelx_estimated_absorpt_t_max   0.842
_shelx_hkl_checksum              37086
_shelx_res_checksum              89773
_shelxl_version_number           .000002012