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_7708643
_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         'C20 H32 Si2 Zr'
_chemical_formula_sum            'C46 H78 Si4 Zr2'
_chemical_formula_weight         453.38
_chemical_name_systematic
1,1-bis(\h5-cyclopentadienyl)-cis-2,5-bis(trimethylsilyl)-1-zirconacyclopent-3-ene
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-10-19 deposited with the CCDC.	2021-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   13.37714(16)
_cell_length_b                   15.7203(2)
_cell_length_c                   23.1966(4)
_cell_measurement_reflns_used    21619
_cell_measurement_temperature    123
_cell_measurement_theta_max      77.17
_cell_measurement_theta_min      3.80
_cell_volume                     4878.07(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_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      123
_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  0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59269
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        64.990
_diffrn_reflns_theta_max         64.990
_diffrn_reflns_theta_min         3.304
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.769
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1884.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.21
_refine_diff_density_min         -1.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0548P)^2^+32.7574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1669
_reflns_d_resolution_high        0.8507
_reflns_number_gt                3847
_reflns_number_total             4279
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1dt03313a2.cif
_cod_data_source_block           ns402ar
_cod_database_code               7708643
_shelx_title                     ' ns402ar'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            622.75
_shelx_f_squared_multiplier      1.000