Redetermination of diaqua[<i>N</i>,<i>N</i>'-bis(3-methoxy-2-oxidobenzylidene)ethylenediamine-κ^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>']manganese(III) perchlorate at 100K
Noor, Shabana; Seidel, Rüdiger W.; Goddard, Richard; Kumar, Sarvendra; Sabir, Suhail; IUCrData 1 (2016) x161735–; doi:10.1107/S2414314616017351

data_1544531
_publ_section_title
;
 Redetermination of
 diaqua[<i>N</i>,<i>N</i>'-bis(3-methoxy-2-oxidobenzylidene)ethylenediamine-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>']manganese(III)
 perchlorate at 100K
;
_journal_coeditor_code           WM4031
_journal_issue                   11
_journal_name_full               IUCrData
_journal_page_first              x161735
_journal_paper_doi               10.1107/S2414314616017351
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          '[Mn (C18 H18 N2 O4) (H2 O)2] Cl O4'
_chemical_formula_moiety         'C18 H22 Mn N2 O6 +, Cl O4 -'
_chemical_formula_sum            'C18 H22 Cl Mn N2 O10'
_chemical_formula_weight         516.76
_chemical_name_systematic
'Diaqua[<i>N</i>,<i>N</i>'-bis(3-methoxy-2-oxidobenzylidene)ethylenediamine-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>']manganese(III) perchlorate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.978(2)
_cell_length_b                   13.2080(19)
_cell_length_c                   22.137(3)
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.8423
_cell_measurement_theta_min      3.2191
_cell_volume                     4087.0(10)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Mach3 APEXII'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            139974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.364
_diffrn_reflns_theta_min         3.085
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  0.97769
_exptl_absorpt_correction_T_min  0.95737
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2013)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.574
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         8570
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+2.5037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                6786
_reflns_number_total             8570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4031sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4086.8(10)
_cod_database_code               1544531
_cod_database_fobs_code          1544531
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.964
_shelx_hkl_checksum              21163
_shelx_res_checksum              26804