Aqua{6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}methanolmanganese(III)) perchlorate hemihydrate
Assey, Gervas; Butcher, Ray J.; Gultneh, Yilma; Acta Crystallographica Section E 66 (2010) m851–m852; doi:10.1107/S1600536810023366

data_2226561
_publ_section_title
;
 Aqua{6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}methanolmanganese(III))
 perchlorate hemihydrate
;
_journal_coeditor_code           JJ2037
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m851
_journal_page_last               m852
_journal_paper_doi               10.1107/S1600536810023366
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Mn (C18 H18 N2 O4) (C H4 O)(H2 O)] Cl O4, 0.5H2 O'
_chemical_formula_moiety         'C19 H24 Mn N2 O6, Cl O4, 0.5(H2 O)'
_chemical_formula_sum            'C19 H25 Cl Mn N2 O10.5'
_chemical_formula_weight         539.80
_chemical_name_systematic
;
Aqua{6,6'-dimethoxy-2,2'-[ethane-1,2-
diylbis(nitrilomethylidyne)]diphenolato}methanolmanganese(III))
perchlorate hemihydrate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 101.324(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.7438(15)
_cell_length_b                   13.3986(9)
_cell_length_c                   16.3266(10)
_cell_measurement_reflns_used    7290
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      32.7210
_cell_measurement_theta_min      4.7343
_cell_volume                     4878.4(6)
_computing_cell_refinement
;
CrysAlis Pro (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis Pro (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis Pro (Oxford Diffraction, 2007)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer with a Ruby (Gemini Mo) detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19303
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.78
_diffrn_reflns_theta_min         4.74
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.844
_refine_ls_abs_structure_details 'Flack (1983), 3800 Friedel pairs'
_refine_ls_abs_structure_Flack   0.254(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         13163
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0828P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                10458
_reflns_number_total             13163
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jj2037.cif
_cod_data_source_block           I
_cod_original_cell_volume        4878.4(5)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2226561
_cod_database_fobs_code          2226561