Di-μ-oxido-bis{bis[<i>N</i>,<i>N</i>'-bis(2-pyridylmethyl)ethane-1,2-diamine]manganese(III,IV)} tris(perchlorate) hexahydrate: clarification of an order–disorder phase transition
Nielsen, Anne; McKenzie, Christine J.; Bond, Andrew D.; Acta Crystallographica Section C 65 (2009) m447–m450; doi:10.1107/S0108270109042127

data_2017401
_publ_section_title
;Di-\m-oxido-bis{bis[<i>N</i>,<i>N</i>'-bis(2-pyridylmethyl)ethane-1,2-diamine]manganese(III,IV)}
 tris(perchlorate) hexahydrate: clarification of an order--disorder phase
 transition
;
_journal_coeditor_code           SF3119
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m447
_journal_page_last               m450
_journal_paper_doi               10.1107/S0108270109042127
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Mn2 O2 (C14 H18 N4)2] (Cl O4)3, 6H2 O'
_chemical_formula_moiety         'C28 H36 Mn2 N8 O2 3+, 3(Cl O4 -), 6(H2 O)'
_chemical_formula_sum            'C28 H48 Cl3 Mn2 N8 O20'
_chemical_formula_weight         1032.97
_chemical_name_systematic
;
Di-\m-oxido-bis{bis[<i>N</i>,<i>N</i>'-bis(2-pyridylpyridyl)ethane-1,2-
diamine]manganese(III,IV)} tris(perchlorate) hexahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.912(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1204(9)
_cell_length_b                   12.2337(7)
_cell_length_c                   23.6514(16)
_cell_measurement_reflns_used    9164
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.18
_cell_volume                     4207.4(5)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker Nonius, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Nonius X8 APEXII CCD area-detector'
_diffrn_measurement_method       'thin-slice \w and \f scans'
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            82186
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.834
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8600
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0826P)^2^+4.7043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                6203
_reflns_number_total             8600
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3119.cif
_cod_data_source_block           I_180K
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2017401
_cod_database_fobs_code          2017401