RuII complexes of 1,2,3-triazoles appended tertiary phosphines, [P(Ph){(o-C6H4)(1,2,3-N3C(Ph)CH}2] and [P(Ph){o-C6H4(CCH)- (1,2,3-N3-Ph)}2]: Highly active catalysts for transfer hydrogenation of carbonyl/nitro compounds and for α–alkylation of ketones
Namdeo, Pavan; sheokand, Sonu; Kote, Basvaraj S.; Radhakrishna, Latchupatula; Kunchur, Harish S.; Saini, Prateek; Ramakrishnan, Srinivasan; Balakrishna, Maravanji Shivaramaiah; Dalton Transactions  (2022) –; doi:10.1039/D2DT00361A

data_7709938
_publ_section_title
;
 RuII complexes of 1,2,3-triazoles appended tertiary phosphines,
 [P(Ph){(o-C6H4)(1,2,3-N3C(Ph)CH}2] and [P(Ph){o-C6H4(CCH)-
 (1,2,3-N3-Ph)}2]: Highly active catalysts for transfer hydrogenation of
 carbonyl/nitro compounds and for \a--alkylation of ketones
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00361A
_journal_year                    2022
_chemical_formula_moiety         'C52 H42 Cl N6 O P2 Ru, Cl, H2 O'
_chemical_formula_sum            'C52 H44 Cl2 N6 O2 P2 Ru'
_chemical_formula_weight         1018.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-25 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5002(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.39402(17)
_cell_length_b                   14.92031(20)
_cell_length_c                   31.2242(4)
_cell_measurement_reflns_used    68681
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.1480
_cell_measurement_theta_min      1.9220
_cell_volume                     5291.82(13)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  70.00   0.50   12.00    --  -20.00   0.00-180.00  360
  2  \w   -110.00  19.00   0.50   12.00    --  -20.00 -72.00  36.00  258
  3  \w   -110.00  19.00   0.50   12.00    --  -20.00 -72.00-180.00  258
  4  \w   -110.00  19.00   0.50   12.00    --  -20.00 -72.00 -36.00  258
  5  \w   -110.00  19.00   0.50   12.00    --  -20.00 -72.00 108.00  258
  6  \w    -58.00  70.00   0.50   12.00    --  -20.00  72.00-180.00  256
  7  \w    -59.00  58.00   0.50   12.00    --  -20.00  72.00 -36.00  234
  8  \w   -110.00  19.00   0.50   12.00    --  -20.00 -72.00-108.00  258
  9  \w    -44.00  67.50   0.50   12.00    --  -20.00  72.00  36.00  223
 10  \w    -11.00  51.00   0.50   12.00    --  -20.00  72.00 108.00  124
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            124950
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.307
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76872
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         9330
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0607P)^2^+9.7454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8317
_reflns_number_total             9330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00361a2.cif
_cod_data_source_block           compound-4_sq
_cod_database_code               7709938
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.922
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C29-C30 \\sim C29-C34A
 with sigma of 0.02
 C29-C34 \\sim C29-C30A
 with sigma of 0.02
 C30-C31 \\sim C34A-C33A
 with sigma of 0.02
 C34-C33 \\sim C30A-C31A
 with sigma of 0.02
 C32-C33 \\sim C32A-C31A
 with sigma of 0.02
 C32-C31 \\sim C32A-C33A
 with sigma of 0.02
 C29-C33 \\sim C29-C31A
 with sigma of 0.04
 C29-C31 \\sim C29-C33A
 with sigma of 0.04
 C30-C32 \\sim C34A-C32A
 with sigma of 0.04
 C34-C32 \\sim C30A-C32A
 with sigma of 0.04
 C33-C31 \\sim C31A-C33A
 with sigma of 0.04
 C21-C22A \\sim C21-C22
 with sigma of 0.02
 C26-C25A \\sim C26-C25
 with sigma of 0.02
 C22A-C23A \\sim C22-C23
 with sigma of 0.02
 C25A-C24A \\sim C25-C24
 with sigma of 0.02
 C23A-C24A \\sim C23-C24
 with sigma of 0.02
 C21-C23A \\sim C21-C23
 with sigma of 0.04
 C26-C24A \\sim C26-C24
 with sigma of 0.04
 C22A-C24A \\sim C22-C24
 with sigma of 0.04
 C25A-C23A \\sim C25-C23
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C22A) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C22A(0.4) H22A(0.4) C25A(0.4) H25A(0.4) C23A(0.4) H23A(0.4)
 C24A(0.4) H24A(0.4) C30(0.6) H30(0.6) C34(0.6) H34(0.6) C32(0.6) H32(0.6)
 C33(0.6) H33(0.6) C31(0.6) H31(0.6) C30A(0.4) H30A(0.4) C31A(0.4) H31A(0.4)
 C32A(0.4) H32A(0.4) C33A(0.4) H33A(0.4) C34A(0.4) H34A(0.4) C22(0.6) H22(0.6)
 C23(0.6) H23(0.6) C24(0.6) H24(0.6) C25(0.6) H25(0.6)
5.a Free rotating group:
 O2(H2A,H2B)
5.b Rotating group:
 O1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C42(H42), C51(H51), C14(H14), C48(H48), C11(H11), C52(H52),
 C39(H39), C28(H28), C38(H38), C49(H49), C50(H50), C8(H8), C43(H43), C46(H46),
 C9(H9), C36(H36), C10(H10), C16(H16), C6(H6), C37(H37), C44(H44), C45(H45),
 C2(H2), C20(H20), C19(H19), C17(H17), C18(H18), C5(H5), C3(H3), C4(H4),
 C22A(H22A), C25A(H25A), C23A(H23A), C24A(H24A), C30(H30), C34(H34), C32(H32),
 C33(H33), C31(H31), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A),
  C22(H22), C23(H23), C24(H24), C25(H25)
;
_shelx_res_checksum              68058
_shelx_hkl_checksum              7268
_shelx_fab_checksum              3350
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;