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_7709936
_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         'C34 H25 N6 P'
_chemical_formula_sum            'C34 H25 N6 P'
_chemical_formula_weight         548.57
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-16
_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                 95.800(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7930(4)
_cell_length_b                   9.8098(4)
_cell_length_c                   28.7992(12)
_cell_measurement_reflns_used    8377
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.4840
_cell_measurement_theta_min      2.4170
_cell_volume                     2752.5(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  19.00   0.50   10.00    --  -20.00 -72.00  36.00  258
  2  \w    -53.00  19.00   0.50   10.00    --  -20.00 -72.00-108.00  144
  3  \w    -87.00  -8.00   0.50   10.00    --  -20.00 -72.00-180.00  158
  4  \w    -30.00  30.00   0.50   10.00    --  -20.00  72.00 108.00  120
;
_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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0302533000
_diffrn_orient_matrix_UB_12      -0.0491882000
_diffrn_orient_matrix_UB_13      0.0159280000
_diffrn_orient_matrix_UB_21      -0.0560497000
_diffrn_orient_matrix_UB_22      0.0066452000
_diffrn_orient_matrix_UB_23      0.0136337000
_diffrn_orient_matrix_UB_31      -0.0352330000
_diffrn_orient_matrix_UB_32      -0.0525746000
_diffrn_orient_matrix_UB_33      -0.0131723000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17055
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.516
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89732
_exptl_absorpt_correction_type   multi-scan
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0407P)^2^+1.1734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3898
_reflns_number_total             4836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00361a2.cif
_cod_data_source_block           compound-1_mo
_cod_database_code               7709936
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.977
_reflns_odcompleteness_completeness 90.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.11
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C2(H2), C10(H10), C8(H8), C22(H22), C16(H16), C33(H33), C11(H11),
 C14(H14), C19(H19), C12(H12), C32(H32), C3(H3), C30(H30), C4(H4), C5(H5),
 C17(H17), C31(H31), C18(H18), C13(H13), C28(H28), C24(H24), C26(H26), C25(H25),
  C27(H27)
;
_shelx_res_checksum              68354
_shelx_hkl_checksum              16460
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.986
_oxdiff_exptl_absorpt_empirical_full_min 0.736