A Neutrally Charged Trimethylmanganese(III) Complex: Synthesis, Characterization, and Disproportionation Chemistry
Stalzer, Madelyn M.; Telser, Joshua; Krzystek, Jurek; Motta, Alessandro; Delferro, Massimiliano; Marks, Tobin J.; Organometallics 35 (2016) 2683–; doi:10.1021/acs.organomet.6b00422

data_4088773
_publ_section_title
;
 A Neutrally Charged Trimethylmanganese(III) Complex: Synthesis,
 Characterization, and Disproportionation Chemistry
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2683
_journal_paper_doi               10.1021/acs.organomet.6b00422
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C9 H25 Mn N2'
_chemical_formula_sum            'C9 H25 Mn N2'
_chemical_formula_weight         216.25
_chemical_name_systematic
trimethyl(N,N,N',N'-tetramethylethylenediamine)manganese
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2016-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 127.2850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5099(3)
_cell_length_b                   13.0628(5)
_cell_length_c                   14.0488(5)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      3.39
_cell_volume                     1242.55(8)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.060
_diffrn_reflns_theta_min         1.559
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0446 before and 0.0288 after correction.
The Ratio of minimum to maximum transmission is 0.8810.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       needle
_exptl_crystal_F_000             472
_exptl_crystal_recrystallization_method 'Recrystallized from pentane at -40C.'
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.413
_exptl_crystal_size_min          0.296
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.0122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3504
_reflns_number_total             3625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00422_si_002.cif
_cod_data_source_block           mnme3
_cod_original_cell_volume        1242.54(8)
_cod_database_code               4088773
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.625
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5234(8) 0.4766(8)
;
_shelx_res_checksum              58438
_shelx_hkl_checksum              88441
_olex2_exptl_crystal_mounting_method 'Mounted in paratone oil. Kept at 100K'
_olex2_submission_special_instructions 'No special instructions were received'