Unusual Rearrangement of Modified PNP Ligand based Ru Complexes Relevant to Alcohol Dehydrogenation Catalysis
Deolka, Shubham; Tarannam, Naziha; Fayzullin, Robert R.; Kozuch, Sebastian; Khaskin, Eugene; Chemical Communications  (2019) –; doi:10.1039/C9CC06024C

data_7124038
_publ_section_title
;
 Unusual Rearrangement of Modified PNP Ligand based Ru Complexes Relevant
 to Alcohol Dehydrogenation Catalysis
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06024C
_journal_year                    2019
_chemical_formula_moiety         'C32 H45 N3 O P2 Ru'
_chemical_formula_sum            'C32 H45 N3 O P2 Ru'
_chemical_formula_weight         650.72
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-01-14 deposited with the CCDC.    2019-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8953(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5325(3)
_cell_length_b                   11.26257(18)
_cell_length_c                   18.0248(3)
_cell_measurement_reflns_used    22879
_cell_measurement_temperature    94(2)
_cell_measurement_theta_max      30.1640
_cell_measurement_theta_min      2.5440
_cell_volume                     3145.90(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics
;
WinGX (Farrugia, 2012); Olex2 (Dolomanov et al., 2009);
ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009)
;
_computing_publication_material  'enCIFer (Allen, 2004)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      94(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54940
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.181
_diffrn_reflns_theta_min         2.235
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015).
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model. Empirical absorption correction using
spherical harmonics, frame scaling and detector area scaling,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_recrystallization_method
'evaporation of a benzene solution at r.t.'
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8387
_refine_ls_number_restraints     492
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+1.5971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7583
_reflns_number_total             8387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06024c2.cif
_cod_data_source_block           jk200
_cod_original_cell_volume        3145.91(9)
_cod_database_code               7124038
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.835
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              26654