Insertion reactions of heteroallenes (CS2 and CO2) into the Ru-H bond of Cp′Ru(PTA)(PR3)H complexes (PTA = 1,3,5-triaza-7-phosphaadamantane)
Lanorio, Jocelyn P.; Frost, Brian J.; Inorganica Chimica Acta 498 (2019) 119138–; doi:10.1016/j.ica.2019.119138

data_1565775
_publ_section_title
;
 Insertion reactions of heteroallenes (CS2 and CO2) into the Ru-H bond of
 Cp&#x2032;Ru(PTA)(PR3)H complexes
 (PTA&#x202F;=&#x202F;1,3,5-triaza-7-phosphaadamantane)
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119138
_journal_paper_doi               10.1016/j.ica.2019.119138
_journal_volume                  498
_journal_year                    2019
_chemical_formula_sum            'C19 H32 Cl2 N6 P2 Ru S2'
_chemical_formula_weight         642.53
_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   difmap
_cell_angle_alpha                90
_cell_angle_beta                 116.4730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1688(4)
_cell_length_b                   21.4324(7)
_cell_length_c                   11.7845(4)
_cell_measurement_reflns_used    8626
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.25
_cell_volume                     2525.12(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34560
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.372
_diffrn_reflns_theta_min         1.900
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.9149
_exptl_absorpt_correction_T_min  0.4581
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.807
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0213
_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^)+(0.0316P)^2^+1.7420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6068
_reflns_number_total             6313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2918-498-119138.cif
_cod_data_source_block           bjf102
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1565775
_shelx_estimated_absorpt_t_min   0.458
_shelx_estimated_absorpt_t_max   0.915