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_7124035
_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 H46 Cl N3 O P2 Ru'
_chemical_formula_sum            'C32 H46 Cl N3 O P2 Ru'
_chemical_formula_weight         687.18
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.4479(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.61551(16)
_cell_length_b                   22.9604(3)
_cell_length_c                   15.1753(3)
_cell_measurement_reflns_used    37339
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      75.1100
_cell_measurement_theta_min      3.5640
_cell_volume                     3229.30(10)
_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      95(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.0359
_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       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57657
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.999
_diffrn_reflns_theta_min         3.583
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.850
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.190
_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            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       plank
_exptl_crystal_F_000             1432
_exptl_crystal_recrystallization_method
'vapor diffusion of hexane into a DCM solution at r.t.'
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.592
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6003
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0833P)^2^+4.9949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5704
_reflns_number_total             6003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06024c2.cif
_cod_data_source_block           jk378a
_cod_original_cell_volume        3229.31(10)
_cod_database_code               7124035
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.190
_shelx_estimated_absorpt_t_max   0.630
_shelx_res_checksum              37991