Pentakis(μ~3~-<i>N</i>,2-dioxidobenzene-1-carboximidato)di-μ~2~-formato-pentakis(1<i>H</i>-imidazole)methanolpentamanganese(III)manganese(II)‒methanol‒water (1/3.36/0.65)
Tigyer, Benjamin R.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 68 (2012) m1521–m1522; doi:10.1107/S1600536812047228

data_2236988
_publ_section_title
;
 Pentakis(\m~3~-<i>N</i>,2-dioxidobenzene-1-carboximidato)di-\m~2~-formato-pentakis(1<i>H</i>-imidazole)methanolpentamanganese(III)manganese(II)--methanol--water
 (1/3.36/0.65)
;
_journal_coeditor_code           PK2457
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1521
_journal_page_last               m1522
_journal_paper_doi               10.1107/S1600536812047228
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Mn6 (C7 H4 N O3)5  (C H O2)2 (C3 H4 N2)5 (C H4 O)], 3.36C H4 O, 0.65H2 O'
_chemical_formula_moiety
'C53 H46 Mn6 N15 O20, 3.36(C H4 O), 0.65(H2 O)'
_chemical_formula_sum            'C56.36 H60.76 Mn6 N15 O24.02'
_chemical_formula_weight         1662.43
_chemical_name_systematic
;
Pentakis(\m~3~-<i>N</i>,2-dioxidobenzene-1-carboximidato)di-\m~2~-formato-
methanolpentakis(1<i>H</i>-imidazole)pentamanganese(III)manganese(II)--
methanol--water (1/3.36/0.65)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 101.8610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2053(12)
_cell_length_b                   24.621(2)
_cell_length_c                   21.491(2)
_cell_measurement_reflns_used    2337
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.61
_cell_measurement_theta_min      2.28
_cell_volume                     6838.1(10)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2012) and <i>CELL_NOW</i> (Sheldrick,
2008<i>b</i>)
;
_computing_data_collection       '<i>APEX2</i> (Bruker, 2012)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2012)'
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2006)
and <i>ORTEP-3</i> for Windows (Farrugia, 2012)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement
;
<i>SHELXL2012</i> (beta 2012-4; Sheldrick, 2012),
<i>SHELXLE Rev582</i> (H\"ubschle <i>et al.</i>, 2011)
;
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008<i>a</i>)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            87486
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         1.576
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>TWINABS</i>; Sheldrick, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3384.9
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.166
_refine_diff_density_min         -0.587
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         17626
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+12.0988P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                14038
_reflns_number_total             17626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2457.cif
_cod_data_source_block           I
_cod_original_cell_volume        6838.0(11)
_cod_database_code               2236988
_cod_database_fobs_code          2236988