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_4088774
_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         'C8 H22 Mn N2'
_chemical_formula_sum            'C8 H22 Mn N2'
_chemical_formula_weight         201.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.9462(8)
_cell_length_b                   11.8486(10)
_cell_length_c                   17.7478(13)
_cell_measurement_reflns_used    5310
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.078
_cell_measurement_theta_min      2.781
_cell_volume                     2301.8(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.14
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10637
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.126
_diffrn_reflns_theta_min         2.781
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS multi-scan absorption correction applied.'
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       needle
_exptl_crystal_F_000             872
_exptl_crystal_preparation
'Crystals handed in the glovebox and mounted in Paratone oil.'
_exptl_crystal_recrystallization_method
'Prepared from a pentane solution at -40C.'
_exptl_crystal_size_max          0.884
_exptl_crystal_size_mid          0.379
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         2285
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0771P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1814
_reflns_number_total             2285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00422_si_003.cif
_cod_data_source_block           mnme2
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               4088774
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.443
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2A-H2B
 1.6 with sigma of 0.01
 C3-H3A = C3-H3B
 0.98 with sigma of 0.01
3. Others
 Fixed Sof: H2A(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 H4C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
4.a Everything fixed:
 H2A, H2B
4.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              97098
_shelx_hkl_checksum              54132
_olex2_exptl_crystal_mounting_method
'Crystal mounted in Paratone oil and after mounting kept at 100K.'
_olex2_submission_special_instructions 'No special instructions were received'