A mesoionic carbene complex of manganese in five oxidation states
Wittwer, Benjamin; Dickmann, Nicole; Berg, Stephan; Leitner, Daniel; Tesi, Lorenzo; Hunger, David; Gratzl, Raphael; van Slageren, Joris; Neuman, Nicolas I.; Munz, Dominik; Hohloch, Stephan; Chemical Communications  (2022) –; doi:10.1039/D2CC00097K

data_7130043
_publ_section_title
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 A mesoionic carbene complex of manganese in five oxidation states
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00097K
_journal_year                    2022
_chemical_formula_moiety         'C64 H76 Mn N14, F6 P'
_chemical_formula_sum            'C64 H76 F6 Mn N14 P'
_chemical_formula_weight         1241.29
_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   geom
_audit_creation_date             2022-01-05
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2022-01-05 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 98.8520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8631(5)
_cell_length_b                   30.7863(10)
_cell_length_c                   17.6752(6)
_cell_measurement_reflns_used    10317
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.99
_cell_volume                     7453.8(4)
_computing_cell_refinement       'Bruker Apex3 suite, 2019'
_computing_data_collection       'Bruker Apex3 suite, 2019'
_computing_data_reduction        'Bruker Apex3 suite, 2019'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            120957
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.990
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0815 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.9317.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         13104
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0844
_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^)+(0.0983P)^2^+26.7546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2168
_refine_ls_wR_factor_ref         0.2336
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10290
_reflns_number_total             13104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00097k2.cif
_cod_data_source_block           sh_0025n_0m
_cod_database_code               7130043
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   'Blessing, 1995'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C28A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26A) \\sim Ueq, Uanis(C27A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C11(H11A,H11B), C7(H7A,H7B), C12(H12A,H12B), C9(H9A,H9B),
 C11A(H11C,H11D), C6A(H6AA,H6AB), C6(H6A,H6B), C12A(H12C,H12D), C10(H10A,H10B),
 C5A(H5AA,H5AB), C8(H8A,H8B), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C7A(H7AA,H7AB),
 C10A(H10C,H10D)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C20(H20), C15A(H15A), C17A(H17A), C15(H15), C20A(H20A), C17(H17),
 C22A(H22A)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C32A(H32A,H32B,H32C), C31(H31A,H31B,
 H31C), C31A(H31D,H31E,H31F), C32(H32D,H32E,H32F), C26A(H26A,H26B,H26C),
 C28A(H28D,H28E,H28F), C26(H26D,H26E,H26F), C30A(H30D,H30E,H30F), C27A(H27A,
 H27B,H27C), C27(H27D,H27E,H27F)
;
_shelx_res_checksum              55152
_shelx_hkl_checksum              23226
_shelx_fab_checksum              37085
_olex2_submission_special_instructions 'No special instructions were received'