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_7130042
_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, 2(F6 P), 2(C3 H6 O)'
_chemical_formula_sum            'C70 H88 F12 Mn N14 O2 P2'
_chemical_formula_weight         1502.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-15
_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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2019-09-15 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.276(3)
_cell_length_b                   21.164(3)
_cell_length_c                   29.506(4)
_cell_measurement_reflns_used    8976
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      1.38
_cell_volume                     14535(3)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart AXS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0873
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            115120
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.701
_diffrn_reflns_theta_min         1.380
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1572 before and 0.0618 after correction.
The Ratio of minimum to maximum transmission is 0.8308.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             6280
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         13805
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0506P)^2^+31.3655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8976
_reflns_number_total             13805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00097k2.cif
_cod_data_source_block           sh_0211_0m
_cod_original_cell_volume        14536(3)
_cod_database_code               7130042
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   'Blessing, 1995'
_olex2_refinement_description
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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. Restrained distances
 C8-C10
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C11A(H11A,H11B), C9(H9A,H9B), C6(H6A,H6B), C5A(H5AA,H5AB), C7A(H7AA,H7AB),
 C9A(H9AA,H9AB), C11(H11C,H11D), C12A(H12A,H12B), C6A(H6AA,H6AB), C5(H5A,H5B),
 C10A(H10A,H10B), C8A(H8AA,H8AB), C7(H7A,H7B), C12(H12C,H12D), C10(H10C,H10D),
 C8(H8A,H8B)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C17A(H17A), C20A(H20A), C22A(H22A), C15(H15), C15A(H15A), C22(H22),
 C20(H20)
4.c Idealised Me refined as rotating group:
 C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32A(H32A,
 H32B,H32C), C26A(H26A,H26B,H26C), C32(H32D,H32E,H32F), C26(H26D,H26E,H26F),
 C27(H27D,H27E,H27F), C201(H20B,H20C,H20D), C31(H31A,H31B,H31C), C28(H28D,H28E,
 H28F), C31A(H31D,H31E,H31F), C202(H20E,H20F,H20G), C30A(H30D,H30E,H30F),
 C101(H10E,H10F,H10G), C102(H10H,H10I,H10J)
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_shelx_res_checksum              34456
_shelx_hkl_checksum              9937
_olex2_submission_special_instructions 'No special instructions were received'