Isonitrile ruthenium and iron PNP complexes: synthesis, characterization and catalytic assessment for base-free dehydrogenative coupling of alcohols.
Nguyen, Duc Hanh; Merel, Delphine; Merle, Nicolas; Trivelli, Xavier; Capet, Frédéric; Gauvin, Régis M; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10067–10081; doi:10.1039/d1dt01722e

data_7707792
_publ_section_title
;
 Isonitrile ruthenium and iron PNP complexes: synthesis, characterization
 and catalytic assessment for base-free dehydrogenative coupling of
 alcohols.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10067
_journal_page_last               10081
_journal_paper_doi               10.1039/d1dt01722e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C32 H51 Br Fe N3 P2, C24 H20 B'
_chemical_formula_sum            'C56 H71 B Br Fe N3 P2'
_chemical_formula_weight         994.66
_chemical_name_systematic        '[Fe(Br)(PhCH2NC)2(PNPH)](BPh4)'
_chemical_properties_physical    Air-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-29 deposited with the CCDC.	2021-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                100.610(2)
_cell_angle_beta                 98.629(2)
_cell_angle_gamma                111.026(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4473(4)
_cell_length_b                   13.7872(5)
_cell_length_c                   17.7984(7)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.31
_cell_volume                     2504.68(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2015 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            79280
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.198
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1040 before and 0.0500 after correction. The Ratio of minimum to maximum transmission is 0.9221. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/pentane'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.324
_refine_diff_density_min         -2.463
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10246
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0148P)^2^+6.2687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8094
_reflns_number_total             10246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01722e2.cif
_cod_data_source_block           mo_dhng056_0m
_cod_depositor_comments
'Adding full bibliography for 7707785--7707792.cif.'
_cod_original_cell_volume        2504.68(16)
_cod_database_code               7707792
_shelx_shelxl_version_number     2018/1
_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. Restrained distances
 C6A-C4A \\sim C6B-C4B \\sim C5A-C4A \\sim C5B-C4B
 with sigma of 0.02
 C6A-C5A \\sim C6B-C5B
 with sigma of 0.04
 C16A-C14A \\sim C16B-C14B \\sim C15A-C14A \\sim C15B-C14B
 with sigma of 0.02
 C16A-C15A \\sim C16B-C15B
 with sigma of 0.04
3. Rigid bond restraints
 C30, C31, C32, C27, C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C6B) = Uanis(C6A)
Uanis(C5B) = Uanis(C5A)
Uanis(C4B) = Uanis(C4A)
Uanis(C16A) = Uanis(C16B)
Uanis(C14A) = Uanis(C14B)
Uanis(C15A) = Uanis(C15B)
5. Others
 Sof(C4B)=Sof(H4B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=Sof(C5B)=Sof(H5BA)=
 Sof(H5BB)=Sof(H5BC)=1-FVAR(1)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=
 Sof(C4A)=Sof(H4A)=FVAR(1)
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C14B)=Sof(H14B)=Sof(C16B)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C14A)=Sof(H14A)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1(H1A), C11(H11), C4B(H4B), C14A(H14A), C4A(H4A), C14B(H14B)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C26(H26A,H26B), C9(H9A,H9B), C10(H10A,H10B), C7(H7A,H7B),
 C8(H8A,H8B)
6.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C36(H36), C37(H37), C42(H42), C44(H44), C43(H43), C52(H52),
 C46(H46), C41(H41), C40(H40), C47(H47), C34(H34), C56(H56), C53(H53), C48(H48),
  C50(H50), C35(H35), C55(H55), C54(H54), C24(H24), C49(H49), C20(H20),
 C21(H21), C22(H22), C23(H23), C28(H28), C32(H32), C29(H29), C31(H31), C30(H30)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C16A(H16A,H16B,H16C),
 C15A(H15A,H15B,H15C), C12(H12A,H12B,H12C), C6A(H6AA,H6AB,H6AC), C5A(H5AA,H5AB,
 H5AC), C6B(H6BA,H6BB,H6BC), C5B(H5BA,H5BB,H5BC), C15B(H15D,H15E,H15F),
 C16B(H16D,H16E,H16F)
;
_shelx_res_checksum              24495
_shelx_hkl_checksum              59674
_olex2_submission_special_instructions 'No special instructions were received'