Tetraethylammonium [12,12-diethyl-2,2,9,9-tetramethyl-1,4,7,10-tetraza-5,6-benzotridecane-3,8,11,13-tetraone(4{-})]oxidomanganate(V)
Berggren, Gustav; Kaynak, Filiz Betul; Anderlund, Magnus F.; Eriksson, Lars; Åkermark, Björn; Acta Crystallographica Section E 63 (2007) m2672–m2673; doi:10.1107/S1600536807047691

data_2215857
_publ_section_title
;Tetraethylammonium
 [12,12-diethyl-2,2,9,9-tetramethyl-1,4,7,10-tetraza-5,6-benzotridecane-3,8,11,13-tetraone(4{-})]oxidomanganate(V)
;
_journal_coeditor_code           CV2305
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2672
_journal_page_last               m2673
_journal_paper_doi               10.1107/S1600536807047691
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C8 H20 N) [Mn (C21 H26 N4 O4) O]'
_chemical_formula_moiety         'C8 H20 N +, C21 H26 Mn N4 O5 -'
_chemical_formula_sum            'C29 H46 Mn N5 O5'
_chemical_formula_weight         599.65
_chemical_name_systematic
;
Tetraethylammonium
[12,12-diethyl-2,2,9,9,-tetramethyl-1,4,7,10-tetraza-5,6-benzotridecane-
3,8,11,13-tetraone(4-)]oxidomanganate(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.024(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2606(11)
_cell_length_b                   15.5269(15)
_cell_length_c                   17.7586(17)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.42
_cell_measurement_theta_min      3.83
_cell_volume                     3087.8(5)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'DIAMOND (Bergerhoff, 1996)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 12
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-3 kappa diffractometer with SapphireIII CCD'
_diffrn_measurement_method       '\w scans at different \f'
_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  0.0777
_diffrn_reflns_av_sigmaI/netI    0.1817
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18232
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.9597
_exptl_absorpt_correction_T_min  0.8985
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                2197
_reflns_number_total             5454
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2305.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2215857
_cod_database_fobs_code          2215857