High-yield synthesis of a unique Mn(iii) siloxide complex through KMnO<sub>4</sub> oxidation of a Mn(ii) precursor.
Lorenz, Volker; Ehle, Sophie; Liebing, Phil; Engelhardt, Felix; Hashemi-Haeri, Haleh; Oehler, Florian; Hinderberger, Dariush; Busse, Sabine; Urbaschok, Jens; Edelmann, Frank T.; Dalton transactions (Cambridge, England : 2003) 47 (2017) 62–66; doi:10.1039/c7dt03500d

data_7045018
_publ_section_title
;
 High-yield synthesis of a unique Mn(iii) siloxide complex through
 KMnO<sub>4</sub> oxidation of a Mn(ii) precursor.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              62
_journal_page_last               66
_journal_paper_doi               10.1039/c7dt03500d
_journal_volume                  47
_journal_year                    2017
_chemical_formula_moiety         'C64 H72 Cl Li2 Mn O10 Si4, 2(C4 H8 O)'
_chemical_formula_sum            'C72 H88 Cl Li2 Mn O12 Si4'
_chemical_formula_weight         1362.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-11-29 deposited with the CCDC.
2017-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.33(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.447(3)
_cell_length_b                   15.753(4)
_cell_length_c                   21.429(4)
_cell_measurement_reflns_used    39936
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.430
_cell_measurement_theta_min      1.938
_cell_volume                     3457.9(15)
_computing_cell_refinement       'X-Area (STOE & Cie, 2002)'
_computing_data_collection       'X-Area (STOE & Cie, 2002)'
_computing_data_reduction        'X-Area and X-Red (STOE & Cie, 2002)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1999)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      ' 289 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            39936
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.430
_diffrn_reflns_theta_min         1.938
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.2595
_exptl_crystal_size_mid          0.1781
_exptl_crystal_size_min          0.0763
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 5576 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1318
_refine_ls_number_reflns         16641
_refine_ls_number_restraints     3816
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+3.3856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.841
_reflns_Friedel_fraction_max     0.770
_reflns_number_gt                15658
_reflns_number_total             16641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03500d2.cif
_cod_data_source_block           fe0072_a
_cod_depositor_comments
'Adding full bibliography for 7045018--7045019.cif.'
_cod_database_code               7045018
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              27906