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_7045019
_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         'C68 H80 Cl2 Li4 Mn O11 Si4, 2(C4 H8 O)'
_chemical_formula_sum            'C76 H96 Cl2 Li4 Mn O13 Si4'
_chemical_formula_weight         1483.48
_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
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-09-07 deposited with the CCDC.
2017-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.723(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   42.7842(12)
_cell_length_c                   13.6537(3)
_cell_measurement_reflns_used    40464
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.084
_cell_measurement_theta_min      1.904
_cell_volume                     7845.7(3)
_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_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.979
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_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40463
_diffrn_reflns_point_group_measured_fraction_full 0.979
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_diffrn_reflns_theta_full        25.084
_diffrn_reflns_theta_max         25.084
_diffrn_reflns_theta_min         2.078
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
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_exptl_crystal_size_min          0.250
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_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         13658
_refine_ls_number_restraints     3594
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9457
_reflns_number_total             13658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03500d2.cif
_cod_data_source_block           li0245
_cod_depositor_comments
'Adding full bibliography for 7045018--7045019.cif.'
_cod_database_code               7045019
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.916
_shelx_res_checksum              10265