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_7709939
_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, 2(C H Cl3), Cl'
_chemical_formula_sum            'C54 H44 Cl8 N6 O P2 Ru'
_chemical_formula_weight         1239.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-06-10
_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                116.271(2)
_cell_angle_beta                 98.231(2)
_cell_angle_gamma                99.230(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2799(3)
_cell_length_b                   14.9883(3)
_cell_length_c                   15.2410(3)
_cell_measurement_reflns_used    30768
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.7670
_cell_measurement_theta_min      2.1620
_cell_volume                     2801.45(12)
_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
_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   9.50   0.50   10.00    --  -20.00 -72.00-108.00  239
  2  \w    -98.00  19.00   0.50   10.00    --  -20.00 -72.00 108.00  234
  3  \w    -59.00  15.50   0.50   10.00    --  -20.00  72.00  36.00  149
  4  \w    -37.50  43.50   0.50   10.00    --  -20.00   0.00  36.00  162
  5  \w    -40.00 -10.00   0.50   10.00    --  -20.00 -72.00-180.00   60
  6  \w    -27.00   3.00   0.50   10.00    --  -20.00 -72.00 -36.00   60
  7  \w    -59.00  61.50   0.50   10.00    --  -20.00  72.00-108.00  241
  8  \w   -110.00   5.00   0.50   10.00    --  -20.00   0.00 108.00  230
  9  \w    -69.00  19.00   0.50   10.00    --  -20.00 -72.00  36.00  176
 10  \w    -58.50   2.00   0.50   10.00    --  -20.00  72.00 -36.00  121
 11  \w    -42.00  -7.00   0.50   10.00    --  -20.00  72.00-180.00   70
 12  \w   -110.00  70.00   0.50   10.00    --  -20.00   0.00 -36.00  360
 13  \w    -59.00  70.00   0.50   10.00    --  -20.00  72.00 108.00  258
 14  \w   -107.00 -69.50   0.50   10.00    --  -20.00   0.00-180.00   75
;
_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      0.0182934000
_diffrn_orient_matrix_UB_12      0.0091640000
_diffrn_orient_matrix_UB_13      0.0498238000
_diffrn_orient_matrix_UB_21      -0.0197944000
_diffrn_orient_matrix_UB_22      -0.0525854000
_diffrn_orient_matrix_UB_23      -0.0151622000
_diffrn_orient_matrix_UB_31      0.0443100000
_diffrn_orient_matrix_UB_32      -0.0111805000
_diffrn_orient_matrix_UB_33      -0.0121954000
_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  0.0787
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65700
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.384
_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    0.763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92515
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0558P)^2^+6.1357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8263
_reflns_number_total             9838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00361a2.cif
_cod_data_source_block           compound-3_mo
_cod_original_cell_volume        2801.45(11)
_cod_database_code               7709939
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.897
_reflns_odcompleteness_completeness 92.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.17
_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.a Rotating group:
 O1(H1A,H1B)
2.b Ternary CH refined with riding coordinates:
 C54(H54), C53(H53)
2.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C16(H16), C7(H7), C3(H3), C21(H21), C2(H2), C5(H5), C34(H34),
 C19(H19), C30(H30), C4(H4), C17(H17), C43(H43), C33(H33), C44(H44), C52(H52),
 C40(H40), C39(H39), C18(H18), C51(H51), C48(H48), C36(H36), C28(H28), C24(H24),
  C50(H50), C31(H31), C45(H45), C49(H49), C32(H32), C38(H38), C46(H46),
 C27(H27), C12(H12), C25(H25), C26(H26), C14(H14), C11(H11), C37(H37), C10(H10),
  C13(H13)
;
_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 1.510
_oxdiff_exptl_absorpt_empirical_full_min 0.805