Pyridine-Based PCP-Ruthenium Complexes: Unusual Structures and Metal-Ligand Cooperation.
Tang, Shan; von Wolff, Niklas; Diskin-Posner, Yael; Leitus, Gregory; Ben-David, Yehoshoa; Milstein, David; Journal of the American Chemical Society 141 (2019) 7554–7561; doi:10.1021/jacs.9b02669

data_4128697
_publ_section_title
;
 Pyridine-Based PCP-Ruthenium Complexes: Unusual Structures and
 Metal-Ligand Cooperation.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7554
_journal_page_last               7561
_journal_paper_doi               10.1021/jacs.9b02669
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C22 H36 Cl N O2 P2 Ru, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C24 H40 Cl N O3 P2 Ru'
_chemical_formula_weight         589.03
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                102.467(2)
_cell_angle_beta                 96.796(2)
_cell_angle_gamma                108.340(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2741(2)
_cell_length_b                   10.9141(2)
_cell_length_c                   16.1941(5)
_cell_measurement_reflns_used    18519
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.7570
_cell_measurement_theta_min      3.7270
_cell_volume                     1327.73(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35734
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.509
_diffrn_reflns_theta_min         3.724
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.596
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         9161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+0.8880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7744
_reflns_number_total             9161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02669_si_002.cif
_cod_data_source_block           4a
_cod_database_code               4128697
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              707
_shelx_hkl_checksum              28124