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_4128695
_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         'C25 H42 Cl N O2 P2 Ru'
_chemical_formula_sum            'C25 H42 Cl N O2 P2 Ru'
_chemical_formula_weight         587.05
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 114.4600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9454(5)
_cell_length_b                   13.3290(5)
_cell_length_c                   15.2365(5)
_cell_measurement_reflns_used    77616
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.216
_cell_volume                     2762.81(17)
_computing_cell_refinement       APEX2
_computing_data_collection       'Collect package Bruker APEX2'
_computing_data_reduction        APEX2
_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      250(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX - II KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            75268
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.343
_diffrn_reflns_theta_min         2.688
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0400P)^2^+2.5381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5633
_reflns_number_total             6868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02669_si_002.cif
_cod_data_source_block           2b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4128695
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.939
_shelx_res_checksum              62697
_shelx_hkl_checksum              14735