Reactions of Five-Membered Zirconacycloalkynes And Zirconacycloallenes with Cp2Zr(H)Cl; Formal Hydrogenation by Metal Hydrides
Suzuki, Noriyuki; Ban, Sayaka; Mochizuki, Ayari; Ito, Saki; Dalton Transactions  (2021) –; doi:10.1039/D1DT03313A

data_7708642
_publ_section_title
;
 Reactions of Five-Membered Zirconacycloalkynes And Zirconacycloallenes
 with Cp2Zr(H)Cl; Formal Hydrogenation by Metal Hydrides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03313A
_journal_year                    2021
_chemical_formula_moiety         'C23 H36 Si2 Zr'
_chemical_formula_sum            'C23 H36 Si2 Zr'
_chemical_formula_weight         459.93
_chemical_name_systematic
1,1-bis(\h5-cyclopentadienyl)-2-triethylsilyl-5-trimethylsilyl-1-zirconacyclopenta-2,3-diene
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-08-22 deposited with the CCDC.	2021-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.5834(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.55776(9)
_cell_length_b                   23.9500(6)
_cell_length_c                   13.75372(17)
_cell_measurement_reflns_used    13675
_cell_measurement_temperature    213
_cell_measurement_theta_max      76.04
_cell_measurement_theta_min      3.67
_cell_volume                     2488.59(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      213
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku XtaLAB P100'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33855
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        68.400
_diffrn_reflns_theta_max         68.400
_diffrn_reflns_theta_min         3.691
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.675
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             968.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.51
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4571
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1251P)^2^+8.0709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2303
_refine_ls_wR_factor_ref         0.2341
_reflns_d_resolution_high        0.8292
_reflns_number_gt                4135
_reflns_number_total             4571
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1dt03313a2.cif
_cod_data_source_block           ns399ar
_cod_database_code               7708642
_shelx_title                     ' xcalibur'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            272.75
_shelx_f_squared_multiplier      1.000