Facile Synthesis and Utilization of Bis(o-phosphinophenyl)zinc as Isolable PZnP-pincer Ligands Enabled by Boron-Zinc Double Transmetallation
Fukuda, Kazuishi; Harada, Takuma; Iwasawa, Nobuharu; Takaya, Jun; Dalton Transactions  (2022) –; doi:10.1039/D2DT01222G

data_7710113
_publ_section_title
;
 Facile Synthesis and Utilization of Bis(o-phosphinophenyl)zinc as
 Isolable PZnP-pincer Ligands Enabled by Boron-Zinc Double
 Transmetallation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01222G
_journal_year                    2022
_chemical_formula_moiety         'C39 H52 O3 P2 Ru Zn'
_chemical_formula_sum            'C39 H52 O3 P2 Ru Zn'
_chemical_formula_weight         797.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-15 deposited with the CCDC.	2022-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5815(2)
_cell_length_b                   11.45430(10)
_cell_length_c                   18.0955(2)
_cell_measurement_reflns_used    15509
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.7370
_cell_measurement_theta_min      4.5530
_cell_volume                     3644.14(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_molecular_graphics    Yadokari-XG
_computing_publication_material  Yadokari-XG
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXS-2013/1
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19129
_diffrn_reflns_point_group_measured_fraction_full 0.734
_diffrn_reflns_point_group_measured_fraction_max 0.733
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.995
_diffrn_reflns_theta_min         4.569
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    5.269
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   1.007(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         4864
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.2049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.417
_reflns_Friedel_fraction_full    0.449
_reflns_Friedel_fraction_max     0.447
_reflns_number_gt                4670
_reflns_number_total             4864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01222g2.cif
_cod_data_source_block           20191004_Fukuda_PZnPCy2P_RuCO3
_cod_database_code               7710113
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.743
_shelx_estimated_absorpt_t_max   0.817
_shelx_res_checksum              36394
_shelx_hkl_checksum              9200