Reaction environment and ligand lability in group 4 Cp2MXY (X, Y = Cl, OtBu) complexes.
Boyde, Nicholas C.; Rightmire, Nicholas R.; Bierschenk, Eric J.; Steelman, Grant W.; Hanusa, Timothy P.; Brennessel, William W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18635–18642; doi:10.1039/c6dt03199d

data_7041080
_publ_section_title
;
 Reaction environment and ligand lability in group 4 Cp2MXY (X, Y = Cl,
 OtBu) complexes.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18635
_journal_page_last               18642
_journal_paper_doi               10.1039/c6dt03199d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C18 H28 Hf O2'
_chemical_formula_sum            'C18 H28 Hf O2'
_chemical_formula_weight         454.89
_chemical_name_common            haneb04
_chemical_name_systematic
bis(cyclopentadienyl)hafnium(bis(tert-butoxide))
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-07-28 deposited with the CCDC.
2016-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4676(7)
_cell_length_b                   8.4676(7)
_cell_length_c                   12.8196(11)
_cell_measurement_reflns_used    4002
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      35.20
_cell_measurement_theta_min      2.88
_cell_volume                     919.17(13)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34629
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.697
_diffrn_reflns_theta_min         1.588
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.677
_exptl_absorpt_correction_T_max  0.4405
_exptl_absorpt_correction_T_min  0.3290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.421
_refine_diff_density_min         -2.269
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
; 
 Flack x determined using 1022 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.023(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2761
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0286P)^2^+3.1716P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                2491
_reflns_number_total             2761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03199d2.cif
_cod_data_source_block           haneb04
_cod_depositor_comments
'Adding full bibliography for 7041078--7041081.cif.'
_cod_original_cell_volume        919.17(17)
_cod_database_code               7041080
_shelx_estimated_absorpt_t_min   0.428
_shelx_estimated_absorpt_t_max   0.549
_shelxl_version_number           2013-2
_shelx_res_checksum              50378