Thermodynamic Analysis of Metal-Ligand Cooperativity of PNP Ru Complexes: Implications for CO<sub>2</sub> Hydrogenation to Methanol and Catalyst Inhibition.
Mathis, Cheryl L.; Geary, Jackson; Ardon, Yotam; Reese, Maxwell S.; Philliber, Mallory A.; VanderLinden, Ryan T.; Saouma, Caroline T.; Journal of the American Chemical Society 141 (2019) 14317–14328; doi:10.1021/jacs.9b06760

data_4128770
_publ_section_title
;
 Thermodynamic Analysis of Metal-Ligand Cooperativity of PNP Ru Complexes:
 Implications for CO<sub>2</sub> Hydrogenation to Methanol and Catalyst
 Inhibition.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14317
_journal_page_last               14328
_journal_paper_doi               10.1021/jacs.9b06760
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C66 H118 K2 N2 O10 P4 Ru2'
_chemical_formula_sum            'C66 H118 K2 N2 O10 P4 Ru2'
_chemical_formula_weight         1503.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 91.2850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3158(5)
_cell_length_b                   12.7484(4)
_cell_length_c                   18.5646(6)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      33.02
_cell_measurement_theta_min      2.29
_cell_volume                     3860.5(2)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER APEX II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            87233
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.168
_diffrn_reflns_theta_min         1.248
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       pyrimid
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.680
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.205
_refine_diff_density_max         2.939
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         29454
_refine_ls_number_restraints     1038
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0676P)^2^+3.2766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1275
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                26036
_reflns_number_total             29454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06760_si_002.cif
_cod_data_source_block           20190329CS_0m
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4128770
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.673
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              35821
_shelx_hkl_checksum              26506