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_7707786
_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, Br'
_chemical_formula_sum            'C32 H51 Br2 Fe N3 P2'
_chemical_formula_weight         755.36
_chemical_name_systematic        '[Fe(Br)(PhCH2NC)2(PNPH)](Br)'
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-07
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   39.4540(9)
_cell_length_b                   39.4540(9)
_cell_length_c                   14.1270(4)
_cell_measurement_reflns_used    8284
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.59
_cell_volume                     19044.2(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.98
_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  0.0865
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            64411
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         1.560
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.341
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1329 before and 0.0607 after correction. The Ratio of minimum to maximum transmission is 0.6580. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       needle
_exptl_crystal_F_000             7020
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/pentane'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         8648
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+10.1109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6301
_reflns_number_total             8648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01722e2.cif
_cod_data_source_block           mo_dhng049_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7707785--7707792.cif.'
_cod_original_cell_volume        19044.2(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7707786
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.531
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Ternary CH refined with riding coordinates:
 C4(H4), C11(H11), C14(H14), C1(H1A)
3.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C18(H18A,H18B), C9(H9A,H9B), C10(H10A,H10B), C7(H7A,H7B),
 C8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C24(H24), C28(H28), C21(H21), C32(H32), C29(H29), C22(H22),
 C23(H23), C31(H31), C30(H30)
3.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C),
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C2(H2A,H2B,H2C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              69457
_shelx_hkl_checksum              45154
_shelx_fab_checksum              4128
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'