Synthesis, structural properties and reactivity of ruthenocene-based pincer Pd(ii) tetrahydroborate.
Safronov, Sergey V.; Gutsul, Evgenii I.; Golub, Igor E.; Dolgushin, Fedor M.; Nelubina, Yulia V.; Filippov, Oleg A.; Epstein, Lina M.; Peregudov, Alexander S.; Belkova, Natalia V.; Shubina, Elena S.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12720–12729; doi:10.1039/c9dt02176k

data_7700679
_publ_section_title
;
 Synthesis, structural properties and reactivity of ruthenocene-based
 pincer Pd(ii) tetrahydroborate.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12720
_journal_page_last               12729
_journal_paper_doi               10.1039/c9dt02176k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C29 H48 O2 P2 Pd Ru, 0.5(C6 H6)'
_chemical_formula_sum            'C32 H51 O2 P2 Pd Ru'
_chemical_formula_weight         737.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2019-01-23 deposited with the CCDC.    2019-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                109.1100(10)
_cell_angle_beta                 105.3890(10)
_cell_angle_gamma                96.9360(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8920(5)
_cell_length_b                   12.0215(6)
_cell_length_c                   15.1339(7)
_cell_measurement_reflns_used    5113
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1596.37(14)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'APEX2 (Bruker, 2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2 DUO 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  0.0429
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21508
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         1.841
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             758
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         9295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0281P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7335
_reflns_number_total             9295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02176k2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7700677--7700680.cif.'
_cod_database_code               7700679
_shelx_estimated_absorpt_t_min   0.845
_shelx_estimated_absorpt_t_max   0.893
_shelxl_version_number           2014/6
_shelx_res_checksum              76645