Pyrazole-pyridine-pyrazole (NNN) ruthenium(II) complex catalyzed acceptorless dehydrogenation of alcohols to aldehydes.
Chen, Yinyin; Cui, Tianhua; Chen, Hua; Li Zheng, Xue; Fu, Haiyan; Li, Ruixiang; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01430d

data_7713755
_publ_section_title
;
 Pyrazole-pyridine-pyrazole (NNN) ruthenium(II) complex catalyzed
 acceptorless dehydrogenation of alcohols to aldehydes.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01430d
_journal_year                    2023
_chemical_formula_moiety         'C63 H55 N5 O2 P2 Ru, Cl, 1[H2O]'
_chemical_formula_sum            'C63 H55 Cl N5 O2 P2 Ru'
_chemical_formula_weight         1112.58
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2frcyj
_audit_creation_date             2023-06-29
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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_audit_update_record
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2023-06-30 deposited with the CCDC.	2023-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.992(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2274(5)
_cell_length_b                   24.983(2)
_cell_length_c                   21.3970(14)
_cell_measurement_reflns_used    5727
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2920
_cell_measurement_theta_min      3.2090
_cell_volume                     5979.0(7)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_unetI/netI     0.1185
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24187
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.981
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.054
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         10456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.1322
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+83.6734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2438
_refine_ls_wR_factor_ref         0.2571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7824
_reflns_number_total             10456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01430d2.cif
_cod_data_source_block           1
_cod_original_cell_volume        5979.1(8)
_cod_database_code               7713755
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.855
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C10(H10), C15(H15), C16(H16), C18(H18),
 C19(H19), C22(H22), C23(H23), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31),
  C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39),
 C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49),
  C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
 C59(H59), C60(H60), C61(H61), C62(H62), C63(H63)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31750
_shelx_fab_checksum              74063
_olex2_submission_special_instructions 'No special instructions were received'