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_7718351
_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
'C91 H63 F39 K Mn N5 O6, 0.5(C7 H8), 0.5(C6 H6)'
_chemical_formula_sum            'C97.5 H70 F39 K Mn N5 O6'
_chemical_formula_weight         2242.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 100.430(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2926(11)
_cell_length_b                   22.9330(12)
_cell_length_c                   21.0751(11)
_cell_measurement_reflns_used    9318
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      59.62
_cell_measurement_theta_min      2.78
_cell_volume                     9645.7(9)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 v2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 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, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Rigaku MicroMax-007HF'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_number            16142
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        64.597
_diffrn_reflns_theta_max         64.596
_diffrn_reflns_theta_min         2.782
_exptl_absorpt_coefficient_mu    2.692
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1289 before and 0.0770 after correction.
 
For component 2:
 wR2(int) was 0.1342 before and 0.0791 after correction.
 The Ratio of minimum to maximum transmission is 0.73.

Final HKLF 4 output contains 284523 reflections, Rint = 0.1313
 (77425 with I > 3sig(I), Rint = 0.0756)
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             4532
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1444
_refine_ls_number_reflns         16142
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0750P)^2^+8.0656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12245
_reflns_number_total             16142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00634a2.cif
_cod_data_source_block           mn_minus1
_cod_depositor_comments
'Adding full bibliography for 7718350--7718351.cif.'
_cod_original_formula_sum        'C97.50 H70 F39 K Mn N5 O6'
_cod_database_code               7718351
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.775
_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. Rigid body (RIGU) restrains
 C102, C103, C104, C105, C106, C101, C107
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C116, C115, C114, C113, C112, C111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F35A)=Sof(F36A)=Sof(F34A)=1-FVAR(1)
 Sof(F36)=Sof(F35)=Sof(F34)=FVAR(1)
 Sof(F20B)=Sof(F21B)=Sof(F19B)=1-FVAR(2)
 Sof(F21A)=Sof(F19A)=Sof(F20A)=FVAR(2)
 Fixed Sof: C102(0.5) H102(0.5) C103(0.5) H103(0.5) C104(0.5) H104(0.5)
 C105(0.5) H105(0.5) C106(0.5) H106(0.5) C101(0.5) C107(0.5) H10A(0.5)
 H10B(0.5) H10C(0.5) C112(0.5) H112(0.5) C111(0.5) H111(0.5) C116(0.5)
 H116(0.5) C115(0.5) H115(0.5) C114(0.5) H114(0.5) C113(0.5) H113(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C125(H12A,H12B), C127(H12C,H12D), C124(H12E,H12F), C126(H12G,H12H), C131(H13A,
 H13B), C123(H12I,H12J), C128(H12K,H12L), C122(H12M,H12N), C121(H12O,H12P)
4.b Aromatic/amide H refined with riding coordinates:
 C75(H75), C82(H82), C86(H86), C73(H73), C45(H45), C22(H22), C26(H26),
 C32(H32), C52(H52), C96(H96), C36(H36), C43(H43), C56(H56), C34(H34), C84(H84),
  C24(H24), C94(H94), C15(H15), C66(H66), C62(H62), C13(H13), C64(H64),
 C92(H92), C54(H54), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106),
  C129(H129), C130(H130), C132(H132), C112(H112), C111(H111), C116(H116),
 C115(H115), C114(H114), C113(H113)
4.c Fitted hexagon refined as free rotating group:
 C102(C103,C104,C105,C106,C101), C112(C111,C116,C115,C114,C113)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C17(H17A,H17B,
 H17C), C49(H49A,H49B,H49C), C18(H18A,H18B,H18C), C107(H10A,H10B,H10C)
;
_shelx_res_checksum              41196
_shelx_hkl_checksum              85331
_olex2_submission_special_instructions 'No special instructions were received'