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_7707785
_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         'C21 H51 B N2 P2 Ru'
_chemical_formula_sum            'C21 H51 B N2 P2 Ru'
_chemical_formula_weight         505.45
_chemical_name_systematic        '[Ru(H)(BH4)(n-BuNC)(PNPH)]'
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2020-05-29 deposited with the CCDC.	2021-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.190(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2348(3)
_cell_length_b                   21.7388(9)
_cell_length_c                   15.2363(6)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      33.04
_cell_measurement_theta_min      2.32
_cell_volume                     2655.57(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (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  0.0346
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77597
_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         33.110
_diffrn_reflns_theta_min         1.662
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1303 before and 0.0457 after correction. The Ratio of minimum to maximum transmission is 0.9232. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         10087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+1.0135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8915
_reflns_number_total             10087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01722e2.cif
_cod_data_source_block           mo_dhng177_0m
_cod_depositor_comments
'Adding full bibliography for 7707785--7707792.cif.'
_cod_database_code               7707785
_shelx_shelxl_version_number     2014/7
_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.a Ternary CH refined with riding coordinates:
 C14(H14), C11(H11), C1(H1A), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C18(H18A,H18B),
 C20(H20A,H20B), C19(H19A,H19B)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C3(H3A,H3B,
 H3C), C6(H6A,H6B,H6C), C21(H21A,H21B,H21C), C13(H13A,H13B,H13C), C2(H2A,H2B,
 H2C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              66845
_shelx_hkl_checksum              29259
_olex2_submission_special_instructions 'No special instructions were received'