Bis(indenyl)hafnium Chemistry: Ligand-Induced Haptotropic Rearrangement and Fundamental Reactivity Studies at a Reduced Hafnium Center
Pun, Doris; Leopold, Scott M.; Bradley, Christopher A.; Lobkovsky, Emil; Chirik, Paul J.; Organometallics 28 (2009) 2471–; doi:10.1021/om900046e

data_4069135
_publ_section_title
;
 Bis(indenyl)hafnium Chemistry: Ligand-Induced Haptotropic Rearrangement
 and Fundamental Reactivity Studies at a Reduced Hafnium Center
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2471
_journal_paper_doi               10.1021/om900046e
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C60 H92 Cl2 Hf2 Na Si8, Na (C4 H10 O2)3'
_chemical_formula_sum            'C72 H122 Cl2 Hf2 Na2 O6 Si8'
_chemical_formula_weight         1782.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.555(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9654(7)
_cell_length_b                   18.6721(7)
_cell_length_c                   16.8308(8)
_cell_measurement_reflns_used    6497
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.01
_cell_measurement_theta_min      2.32
_cell_volume                     4340.0(3)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36740
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    2.616
_exptl_absorpt_correction_T_max  0.6950
_exptl_absorpt_correction_T_min  0.5075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details          ' '
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         8807
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.566
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0689
_reflns_number_gt                5972
_reflns_number_total             8807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900046e_si_003.cif
_cod_data_source_block           dp13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4069135