μ~3~-Acetato-μ~2~-acetato-(dimethylformamide)pentakis(μ-<i>N</i>,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1<i>H</i>-imidazole)pentamanganese(III)manganese(II)‒diethyl ether‒dimethylformamide‒methanol‒water (1/1/1/1/0.49)
Tigyer, Benjamin R.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 69 (2013) m393–m394; doi:10.1107/S1600536813015857

data_2238198
_publ_section_title
;
 \m~3~-Acetato-\m~2~-acetato-(dimethylformamide)pentakis(\m-<i>N</i>,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1<i>H</i>-imidazole)pentamanganese(III)manganese(II)--diethyl
 ether--dimethylformamide--methanol--water (1/1/1/1/0.49)
;
_journal_coeditor_code           JJ2164
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m393
_journal_page_last               m394
_journal_paper_doi               10.1107/S1600536813015857
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac
;
[Mn6 (C7 H4 N O3)5 (C2 H3 O2)2 (C4 H6 N2)4.62 (C3 H7 N O)1.38], C4 H10 O,
C3 H7 N O, C H4 O, 0.49H2 O
;
_chemical_formula_moiety
;
C61.61958 H63.38042 Mn6 N15.61958 O20.38042, 0.49064(H2 O), C3 H7 N O, C4 H10 O,
C H4 O
;
_chemical_formula_sum            'C69.61958 H85.3617 Mn6 N16.61958 O23.87106'
_chemical_formula_weight         1866.61
_chemical_name_systematic
;\m~3~-Acetato-\m~2~-acetato-(dimethylformamide)pentakis(\m-<i>N</i>,2-dioxidobenzene-1-carboximidato)pentakis(1-methyl-1<i>H</i>-imidazole)pentamanganese(III)manganese(II)--diethyl
ether--dimethylformamide--methanol--water (1/1/1/1/0.49)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                102.166(4)
_cell_angle_beta                 96.726(4)
_cell_angle_gamma                107.496(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4181(8)
_cell_length_b                   17.0108(11)
_cell_length_c                   20.6627(13)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.6399
_cell_measurement_theta_min      2.1967
_cell_volume                     3992.4(5)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    '<i>Mercury</i> (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  '<i>publCIF</i> (Westrip, 2010)'
_computing_structure_refinement
;
SHELXL2012 (Sheldrick, 2008<i>a</i>) and
<i>SHELXLE Rev600</i> (H\"ubschle <i>et al.</i>, 2011)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008<i>a</i>)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1340
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            56608
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.300
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.746457
_exptl_absorpt_correction_T_min  0.543819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>TWINABS</i>; Sheldrick, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920.8
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.073
_refine_diff_density_min         -1.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1146
_refine_ls_number_reflns         18890
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.0868
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+15.4132P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2319
_reflns_number_gt                13018
_reflns_number_total             18890
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jj2164.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C69.61958 H85.36170 Mn6 N16.61958 O23.87106'
_cod_database_code               2238198
_cod_database_fobs_code          2238198
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.864
_shelx_hkl_checksum              8928
_shelx_res_checksum              15261
_shelxl_version_number           .000002012