Di- and Tetrametallic Hafnocene Oxamidides Prepared from CO-Induced N2Bond Cleavage and Thermal Rearrangement to Hafnocene Cyanide Derivatives
Semproni, Scott P.; Margulieux, Grant W.; Chirik, Paul J.; Organometallics 31 (2012) 6278–; doi:10.1021/om3005542

data_4079187
_publ_section_title
;
 Di- and Tetrametallic Hafnocene Oxamidides Prepared from CO-Induced
 N2Bond Cleavage and Thermal Rearrangement to Hafnocene Cyanide
 Derivatives
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6278
_journal_paper_doi               10.1021/om3005542
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C50 H76 Hf2 N2 O3.92 Si2'
_chemical_formula_weight         1181.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 133.6660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.222(3)
_cell_length_b                   9.6875(9)
_cell_length_c                   22.409(2)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.29
_cell_volume                     4903.0(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_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  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20184
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    4.325
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             2373.6
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0083P)^2^+15.9896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0390
_refine_ls_wR_factor_ref         0.0394
_reflns_number_gt                5112
_reflns_number_total             5508
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3005542_si_003.cif
_cod_data_source_block           sps70
_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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4079187