Di-μ-oxido-bis[(1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')dimanganese(III,IV)] bis(tetraphenylborate) chloride acetonitrile disolvate
Olmstead, Marilyn M.; Boyce, David W.; Bria, Lauren E.; Acta Crystallographica Section E 67 (2011) m824–m825; doi:10.1107/S1600536811019829

data_2230686
_publ_section_title
;
 Di-\m-oxido-bis[(1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')dimanganese(III,IV)]
 bis(tetraphenylborate) chloride acetonitrile disolvate
;
_journal_coeditor_code           HG5039
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m824
_journal_page_last               m825
_journal_paper_doi               10.1107/S1600536811019829
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Mn2 O2 (C10 H24 N4)2] (C24 H20 B)2 Cl, 2C2 H3 N'
_chemical_formula_moiety
'C20 H48 Mn2 N8 O2 3+, 2(C24 H20 B -), Cl -, 2(C2 H3 N)'
_chemical_formula_sum            'C72 H94 B2 Cl Mn2 N10 O2'
_chemical_formula_weight         1298.52
_chemical_name_systematic
;
Di-\m-oxido-bis[(1,4,8,11-tetraazacyclotetradecane-
\k^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')dimanganese(III,IV)]
bis(tetraphenylborate) chloride acetonitrile disolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                104.136(3)
_cell_angle_beta                 97.697(3)
_cell_angle_gamma                107.627(3)
_cell_formula_units_Z            1
_cell_length_a                   11.437(2)
_cell_length_b                   11.713(2)
_cell_length_c                   13.967(3)
_cell_measurement_reflns_used    3568
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.76
_cell_volume                     1684.9(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       \w
_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  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17931
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             689
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.806
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6092
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+1.3759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1726
_reflns_number_gt                4083
_reflns_number_total             6092
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg5039.cif
_cod_data_source_block           I
_cod_database_code               2230686
_cod_database_fobs_code          2230686