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_4128699
_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 H43 N O2 P2 Ru'
_chemical_formula_sum            'C25 H43 N O2 P2 Ru'
_chemical_formula_weight         552.61
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.982(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2611(5)
_cell_length_b                   15.6139(5)
_cell_length_c                   15.0481(6)
_cell_measurement_reflns_used    18746
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.4850
_cell_measurement_theta_min      3.8430
_cell_volume                     2707.43(19)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35826
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.709
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.734
_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            yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.930
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         8242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+1.5634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7217
_reflns_number_total             8242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02669_si_002.cif
_cod_data_source_block           8b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4128699
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              30740
_shelx_hkl_checksum              29063