Novel ruthenium complexes bearing bipyridine-based and N-heterocyclic carbene-supported pyridine (NCN) ligands: the influence of ligands on catalytic transfer hydrogenation of ketones.
Piyasaengthong, Akkharadet; Williams, Luke J.; Yufit, Dmitry S.; Walton, James W.; Dalton transactions (Cambridge, England : 2003) 51 (2021) 340–351; doi:10.1039/d1dt03240b

data_7708976
_publ_section_title
;
 Novel ruthenium complexes bearing bipyridine-based and N-heterocyclic
 carbene-supported pyridine (NCN) ligands: the influence of ligands on
 catalytic transfer hydrogenation of ketones.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              340
_journal_page_last               351
_journal_paper_doi               10.1039/d1dt03240b
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety         'C25 H29 N4 Ru, C H2 Cl2, F6 P'
_chemical_formula_sum            'C26 H31 Cl2 F6 N4 P Ru'
_chemical_formula_weight         716.49
_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             2020-08-27
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6371(4)
_cell_length_b                   14.0622(5)
_cell_length_c                   16.8293(6)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      30.63
_cell_measurement_theta_min      2.17
_cell_volume                     2982.24(18)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'Bruker PHOTON III MM CPAD'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CPA sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w- and \f-scan'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44067
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.170
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0 microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0607 before and 0.0488 after correction.
The Ratio of minimum to maximum transmission is 0.8566.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8700
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0700P)^2^+8.6800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6563
_reflns_number_total             8700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03240b2.cif
_cod_data_source_block           5_20srv194
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7708973--7708976.cif.
;
_cod_database_code               7708976
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.887
_computing_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_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
 P1A-F6A \\sim P1-F2 \\sim P1A-F2A \\sim P1A-F5A \\sim P1-F5 \\sim P1-F3 \\sim
P1A-F3A \\sim P1-F6 \\sim P1-F4
 \\sim P1-F1 \\sim P1A-F1 \\sim P1A-F4A
 with sigma of 0.003
3. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4A)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C21A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C18(0.5) C19(0.5) C20(0.5) C16(0.5) C17(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5)
 H25B(0.5) H25C(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C18A(0.5) C19A(0.5) C20A(0.5) C16A(0.5) C17A(0.5)
 C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5) C24A(0.5) H24D(0.5) H24E(0.5)
 H24F(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5) C21A(0.5) H21D(0.5)
 H21E(0.5) H21F(0.5) C22A(0.5) H22D(0.5) H22E(0.5) H22F(0.5) P1(0.5) P1A(0.5)
 F2(0.5) F2A(0.5) F3(0.5) F3A(0.5) F4(0.5) F4A(0.5) F5(0.5) F5A(0.5) F6(0.5)
 F6A(0.5)
5.a Riding coordinates:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F),
 C25A(H25D,H25E,H25F), C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C10(H10A,H10B), C1S(H1SA,H1SB)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15)
5.d Cp* refined as free rotating group:
 C18(C19,C20,C16,C17,C23,C24,C25,C21,C22), C18A(C19A,C20A,C16A,C17A,C23A,C24A,
 C25A,C21A,C22A)
;
_olex2_submission_special_instructions 'No special instructions were received'