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_7713756
_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         'C49 H43 Cl N5 P2 Ru, Cl, 2(H2 O)'
_chemical_formula_sum            'C49 H46 Cl2 N5 O2 P2 Ru'
_chemical_formula_weight         970.82
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2ggn2p
_audit_creation_date             2023-06-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-30 deposited with the CCDC.	2023-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.851(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8398(8)
_cell_length_b                   21.1962(19)
_cell_length_c                   19.7092(17)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      30.973
_cell_measurement_theta_min      2.183
_cell_volume                     4928.5(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      138.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39187
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.922
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1045 before and 0.0749 after correction.
The Ratio of minimum to maximum transmission is 0.8212.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       block
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.633
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         8644
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1203P)^2^+21.2256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7514
_reflns_number_total             8644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01430d2.cif
_cod_data_source_block           mo_lrx_cyy_1_100k_0m_a
_cod_database_code               7713756
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.905
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Free rotating group:
 O4(H4A,H4B), O(HA,HB)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3A), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21),
  C24(H24), C25(H25), C26(H26), C29(H29), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45),
  C46(H46), C47(H47), C48(H48), C49(H49)
3.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              81630
_olex2_submission_special_instructions 'No special instructions were received'