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_7708973
_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
'C30 H27 Cl N4 P Ru, Cl, 2(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C32 H36 Cl2 N4 O2.5 P Ru'
_chemical_formula_weight         719.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-26
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.531(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.9245(9)
_cell_length_b                   11.0559(5)
_cell_length_c                   30.7401(14)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.32
_cell_measurement_theta_min      2.34
_cell_volume                     6457.0(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 C7 MM CPAD'
_diffrn_detector_area_resol_mean 54.8
_diffrn_detector_type            'CPA sensor'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            55339
_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         29.996
_diffrn_reflns_theta_min         2.131
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0720 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.9347.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       plank
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.014
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         9406
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0475P)^2^+10.7482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7267
_reflns_number_total             9406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03240b2.cif
_cod_data_source_block           2_21srv181
_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_original_formula_sum        'C32 H36 Cl2 N4 O2.50 P Ru'
_cod_database_code               7708973
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.910
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N1-H1 = N4-H4
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C5(H5), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
5.d Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
5.e Idealised tetrahedral OH refined as rotating group:
 O1S(H1S), O2S(H2S)
;
_olex2_submission_special_instructions 'No special instructions were received'