A mixed isocyanide Mn(I) complex and its reduction to a metallate.
Claude, Guilhem; Ellwanger, Mathias A.; Grippo, Adam; Hernandez, Ritchie; Figueroa, Joshua R.; Abram, Ulrich; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6025–6028; doi:10.1039/d5dt00634a

data_7718350
_publ_section_title
;
 A mixed isocyanide Mn(I) complex and its reduction to a metallate.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6025
_journal_page_last               6028
_journal_paper_doi               10.1039/d5dt00634a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C79 H42 Br F39 Mn N5, C3.5 H4'
_chemical_formula_sum            'C82.5 H46 Br F39 Mn N5'
_chemical_formula_weight         1983.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-16 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                87.5900(10)
_cell_angle_beta                 88.9030(10)
_cell_angle_gamma                83.9410(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7013(3)
_cell_length_b                   13.2387(3)
_cell_length_c                   24.4356(6)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    126
_cell_measurement_theta_max      77.28
_cell_measurement_theta_min      3.62
_cell_volume                     4081.80(17)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      126.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47210
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.420
_diffrn_reflns_theta_min         1.810
_exptl_absorpt_coefficient_mu    3.142
_exptl_absorpt_correction_T_max  0.5368
_exptl_absorpt_correction_T_min  0.4065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0873 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.7573.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             1974
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1420
_refine_ls_number_reflns         16626
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0827P)^2^+2.8798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14480
_reflns_number_total             16626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00634a2.cif
_cod_data_source_block           mn_plus1
_cod_depositor_comments
'Adding full bibliography for 7718350--7718351.cif.'
_cod_original_formula_sum        'C82.50 H46 Br F39 Mn N5'
_cod_database_code               7718350
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.542
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F31B-C97 \\sim F31A-C97 \\sim F32B-C97 \\sim F15-C97 \\sim F33A-C97 \\sim
F33B-C97
 with sigma of 0.02
 F18B-C58 \\sim F18A-C58 \\sim F16B-C58 \\sim F16A-C58 \\sim F17B-C58 \\sim
F17A-C58
 with sigma of 0.02
 C48B-C40 \\sim C48A-C40 \\sim C49A-C40 \\sim C49B-C40 \\sim C47A-C40 \\sim
C47B-C40
 with sigma of 0.02
 F26A-C68 \\sim F25A-C68 \\sim F27A-C68
 with sigma of 0.02
 F26A-C68 \\sim F26B-C68 \\sim F25A-C68 \\sim F25B-C68 \\sim F27B-C68 \\sim
F27A-C68
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F27B) = Uanis(F26B)
4. Rigid body (RIGU) restrains
 C65, C68, F25A, F25B, F27B, F27A, F26A, F26B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55, C58, F17A, F17B, F16A, F16B, F18A, F18B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C40, C49A, C49B, C47A, C47B, C48A, C48B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C10, C19B, C19A, C18B, C17, C18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C68, F26A, F26B, F25A, F25B, F27B, F27A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=1-FVAR(1)
 Sof(C48B)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C47B)=Sof(H47A)=Sof(H47B)=
 Sof(H47C)=Sof(C49B)=Sof(H49A)=Sof(H49B)=Sof(H49C)=FVAR(1)
 Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C18B)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=1-FVAR(2)
 Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C18A)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=FVAR(2)
 Sof(F32B)=Sof(F31B)=Sof(F33A)=1-FVAR(3)
 Sof(F33B)=Sof(F31A)=Sof(F15)=FVAR(3)
 Sof(F18B)=Sof(F17B)=Sof(F16B)=1-FVAR(4)
 Sof(F18A)=Sof(F17A)=Sof(F16A)=FVAR(4)
 Sof(F27B)=Sof(F26B)=Sof(F25B)=1-FVAR(5)
 Sof(F27A)=Sof(F26A)=Sof(F25A)=FVAR(5)
 Sof(F7B)=Sof(C37B)=Sof(F9B)=Sof(F8B)=1-FVAR(6)
 Sof(F9A)=Sof(F8A)=Sof(F7A)=Sof(C37A)=FVAR(6)
 Sof(F14B)=Sof(F13B)=Sof(F15B)=1-FVAR(7)
 Sof(F14A)=Sof(F15A)=Sof(F13A)=FVAR(7)
 Sof(F12A)=Sof(F11A)=Sof(F10A)=1-FVAR(8)
 Sof(F10B)=Sof(F11B)=Sof(F12B)=FVAR(8)
 Sof(F21B)=Sof(F19B)=Sof(F20B)=1-FVAR(9)
 Sof(F21A)=Sof(F19A)=Sof(F20A)=FVAR(9)
 Fixed Sof: H102(0.5) C103(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C52(H52), C13(H13), C73(H73), C15(H15), C22(H22), C62(H62),
 C75(H75), C54(H54), C26(H26), C34(H34), C92(H92), C96(H96), C86(H86), C82(H82),
  C56(H56), C24(H24), C43(H43), C94(H94), C84(H84), C45(H45), C64(H64),
 C32(H32), C66(H66), C102(H102), C101(H101), C100(H100)
6.b Idealised Me refined as rotating group:
 C19A(H19A,H19B,H19C), C17(H17A,H17B,H17C), C48B(H48A,H48B,H48C), C18A(H18A,
 H18B,H18C), C47B(H47A,H47B,H47C), C49B(H49A,H49B,H49C), C48A(H48D,H48E,H48F),
 C47A(H47D,H47E,H47F), C49A(H49D,H49E,H49F), C19B(H19D,H19E,H19F), C18B(H18D,
 H18E,H18F), C103(H10A,H10B,H10C)
;
_shelx_res_checksum              47757
_shelx_hkl_checksum              33649
_olex2_date_sample_data_collection 2023-04-13
_olex2_date_sample_submission    2023-04-13
_olex2_exptl_crystal_mounting_method
'The crystal picked from perfluoro-oil and mounted on a MiTeGen MicroLoop. '
_olex2_submission_special_instructions 'No special instructions were received'