A Redox-active Manganate(0) Dicarbene Metalloradical
Karagiannis, Ageliki; Tyryshkin, Alexei M.; Lalancette, Roger A.; Spasyuk, Denis M.; Washington, Asmaa; Prokopchuk, Demyan E.; Chemical Communications  (2022) –; doi:10.1039/D2CC04677F

data_7130893
_publ_section_title
;
 A Redox-active Manganate(0) Dicarbene Metalloradical
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04677F
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_sum            'C47 H68 B K Mn N6 O9'
_chemical_formula_weight         965.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-08 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.789(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1465(8)
_cell_length_b                   16.0225(15)
_cell_length_c                   20.4295(6)
_cell_measurement_reflns_used    14776
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.096
_cell_measurement_theta_min      3.507
_cell_volume                     4853.3(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28203
_diffrn_reflns_point_group_measured_fraction_full 0.737
_diffrn_reflns_point_group_measured_fraction_max 0.691
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.380
_diffrn_reflns_theta_min         3.535
_exptl_absorpt_coefficient_mu    3.460
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       plate
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.015(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         7043
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0630P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.431
_reflns_Friedel_fraction_full    0.475
_reflns_Friedel_fraction_max     0.417
_reflns_number_gt                6323
_reflns_number_total             7043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04677f3.cif
_cod_data_source_block           211028RAL_AK_378_100K
_cod_original_cell_volume        4853.4(5)
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               7130893
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.757
_oxdiff_exptl_absorpt_empirical_full_max 1.186
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              4744
_shelx_hkl_checksum              57980