Influence of triphosphine ligand coordination geometry in Mn(I) hydride complexes [(P<sup>∩</sup>P<sup>∩</sup>P)(CO)<sub>2</sub>MnH] on their kinetic hydricity.
Kovalenko, Sergey A.; Gulyaeva, Ekaterina S.; Osipova, Elena S.; Filippov, Oleg A.; Danshina, Anastasia A.; Vendier, Laure; Kireev, Nikolay V.; Godovikov, Ivan A.; Canac, Yves; Valyaev, Dmitry A.; Belkova, Natalia V.; Shubina, Elena S.; Dalton transactions (Cambridge, England : 2003) 54 (2024) 122–132; doi:10.1039/d4dt02496f

data_7717420
_publ_section_title
;
 Influence of triphosphine ligand coordination geometry in Mn(I) hydride
 complexes
 [(P<sup>&#x2229;</sup>P<sup>&#x2229;</sup>P)(CO)<sub>2</sub>MnH] on their
 kinetic hydricity.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              122
_journal_page_last               132
_journal_paper_doi               10.1039/d4dt02496f
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C45 H42 Mn N O2 P3, C H2 Cl2, B F4'
_chemical_formula_sum            'C46 H44 B Cl2 F4 Mn N O2 P3'
_chemical_formula_weight         948.38
_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
_audit_creation_date             2024-07-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-17 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                80.196(6)
_cell_angle_beta                 76.870(6)
_cell_angle_gamma                80.423(4)
_cell_formula_units_Z            2
_cell_length_a                   9.1917(8)
_cell_length_b                   14.0017(14)
_cell_length_c                   17.7856(16)
_cell_measurement_reflns_used    5121
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.30
_cell_volume                     2177.1(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.1479
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16953
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.029
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1043 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.8291.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.785
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         9048
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1631
_refine_ls_R_factor_gt           0.1107
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+24.4673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2564
_refine_ls_wR_factor_ref         0.2774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5564
_reflns_number_total             9048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02496f3.cif
_cod_data_source_block           1MeCN+
_cod_depositor_comments
'Adding full bibliography for 7717420--7717424.cif.'
_cod_database_code               7717420
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C45-C40 \\sim C45'-C40
 with sigma of 0.02
 C44-C45 \\sim C44'-C45'
 with sigma of 0.02
 C44-C43 \\sim C44'-C43'
 with sigma of 0.02
 Cl3S-C1S \\sim Cl1S-C1S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C40) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C42) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C44) = Uanis(C44')
Uanis(C43) = Uanis(C43')
Uanis(C45) = Uanis(C45')
Uanis(Cl3S) = Uanis(Cl1S)
4. Others
 Sof(H42A)=Sof(C43')=Sof(H43')=Sof(C44')=Sof(H44')=Sof(C45')=Sof(H45')=1-FVAR(1)
 Sof(H42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=FVAR(1)
 Sof(H1SC)=Sof(H1SD)=Sof(Cl1S)=1-FVAR(2)
 Sof(H1SA)=Sof(H1SB)=Sof(Cl3S)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C33(H33A,H33B), C1S(H1SA,H1SB), C1S(H1SC,H1SD)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C35(H35), C36(H36), C37(H37),
 C38(H38), C39(H39), C41(H41), C42(H42), C42(H42A), C43(H43), C44(H44),
 C45(H45), C43'(H43'), C44'(H44'), C45'(H45')
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              99293
_shelx_hkl_checksum              807
_olex2_submission_special_instructions 'No special instructions were received'