Tris(μ~2~-methanolato)-μ~3~-oxido-tris{[(<i>E</i>)-4-chloro-2-({[2-(pyridin-2-yl)ethyl]imino}methyl)phenolato]manganese(III)} perchlorate‒dichloromethane‒diethyl ether (1/1.1/0.9)
Egekenze, Rita; Gultneh, Yilma; Butcher, Ray J.; Acta Crystallographica Section E 73 (2017) 1113–1116; doi:10.1107/S2056989017008982

data_2242180
_publ_section_title
;
 Tris(\m~2~-methanolato)-\m~3~-oxido-tris{[(<i>E</i>)-4-chloro-2-({[2-(pyridin-2-yl)ethyl]imino}methyl)phenolato]manganese(III)}
 perchlorate--dichloromethane--diethyl ether (1/1.1/0.9)
;
_journal_coeditor_code           ZL2705
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1113
_journal_page_last               1116
_journal_paper_doi               10.1107/S2056989017008982
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac
'[Mn3 (C14 H12 Cl N2 O)3 (C H3 O)3 O] Cl O4, 1.096C H2 Cl2, 0.906C4 H10 O'
_chemical_formula_moiety
'C45 H45 Cl3 Mn3 N6 O7 +, Cl O4 -, 1.096(C H2 Cl2), 0.904(C4 H10 O)'
_chemical_formula_sum            'C49.71 H56.23 Cl6.19 Mn3 N6 O11.9'
_chemical_formula_weight         1312.41
_chemical_name_systematic
;Tris(\m~2~-methanolato)-\m~3~-oxido-tris[(<i>E</i>)-4-chloro-2-({[2-(pyridin-2-yl)ethyl]imino}methyl)phenolato]manganese(III)
perchlorate--dichloromethane--diethyl ether (1/1.096/0.906)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 100.0727(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0002(3)
_cell_length_b                   19.3890(2)
_cell_length_c                   19.1631(3)
_cell_measurement_reflns_used    18751
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      40.9251
_cell_measurement_theta_min      2.9655
_cell_volume                     5853.30(16)
_computing_cell_refinement
;
CrysAlis PRO (Agilent 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent 2012)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Agilent Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            108163
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         41.025
_diffrn_reflns_theta_min         3.013
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent 2012)
;
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.3214
_exptl_crystal_size_mid          0.2742
_exptl_crystal_size_min          0.1755
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.775
_refine_ls_extinction_coef       0.00127(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         37613
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+3.6302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1664
_reflns_number_gt                23139
_reflns_number_total             37613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2705sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        5853.31(16)
_cod_original_formula_sum        'C49.71 H56.23 Cl6.19 Mn3 N6 O11.90'
_cod_database_code               2242180
_shelx_hkl_checksum              23730
_shelx_res_checksum              49412
_cod_database_fobs_code 2242180