Crystal structure of bis(2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)manganese(IV) 0.39-hydrate
Buvaylo, Elena A.; Vassilyeva, Olga Yu.; Skelton, Brian W.; Acta Crystallographica Section E 71 (2015) 1307–1310; doi:10.1107/S2056989015018551

data_2241195
_publ_section_title
;
 Crystal structure of
 bis(2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)manganese(IV)
 0.39-hydrate
;
_journal_coeditor_code           SJ5481
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1307
_journal_page_last               1310
_journal_paper_doi               10.1107/S2056989015018551
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Mn (C12 H15 N O5)2] , 0.39H2 O'
_chemical_formula_moiety         'C24 H30 Mn N2 O10, 0.39(H2 O)'
_chemical_formula_sum            'C24 H30.78 Mn N2 O10.39'
_chemical_formula_weight         568.46
_chemical_name_systematic
'Bis(2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)manganese(IV) 0.39 hydrate'
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0953(2)
_cell_length_b                   8.0953(2)
_cell_length_c                   37.568(2)
_cell_measurement_reflns_used    2851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.5978
_cell_measurement_theta_min      3.5266
_cell_volume                     2461.98(16)
_computing_cell_refinement
;
<i>CrysAlis Pro</i> (Agilent, 2014)
;
_computing_data_collection
;
<i>CrysAlis Pro</i> (Agilent, 2014)
;
_computing_data_reduction
;
<i>CrysAlis Pro</i> (Agilent, 2014)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL-2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1993)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.103
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            18553
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.705
_diffrn_reflns_theta_min         4.708
_exptl_absorpt_coefficient_mu    4.92
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[<i>CrysAlis Pro</i> (Agilent, 2014)
     using an expression derived by Clark & Reid (1995)]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       plate
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.342
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 584 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al</i>., 2013).
;
_refine_ls_abs_structure_Flack   -0.007(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+1.3653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1358
_reflns_number_gt                1885
_reflns_number_total             2214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5481sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2461.97(18)
_cod_database_code               2241195
_shelx_hkl_checksum              73442
_shelx_res_checksum              3915
_cod_database_fobs_code 2241195