Zirconium and hafnium (1-pyridinio)imido complexes: functionalized terminal hydrazinediido analogues
Herrmann, Heike; Gehrmann, Thorsten; Wadepohl, Hubert; Gade, Lutz H.; Dalton Transactions  (2008) 6231–6241; doi:10.1039/b807808d

data_7004478
_publ_section_title
;
 Zirconium and hafnium (1-pyridinio)imido complexes: functionalized
 terminal hydrazinediido analogues
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              6231
_journal_page_last               6241
_journal_paper_doi               10.1039/b807808d
_journal_year                    2008
_chemical_formula_sum            'C39 H59 F3 Hf N6 O3 S Si2'
_chemical_formula_weight         983.65
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tg2b
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.6470(10)
_cell_angle_beta                 82.7360(10)
_cell_angle_gamma                75.6280(10)
_cell_formula_units_Z            4
_cell_length_a                   10.8631(7)
_cell_length_b                   13.8086(9)
_cell_length_c                   31.0427(19)
_cell_measurement_temperature    100(2)
_cell_volume                     4459.4(5)
_computing_cell_refinement       'SAINT (Bruker AXS, 1997-2006)'
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2006)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens, 1999-2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector (Bruker AXS Smart 1000)'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            111883
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.66
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.494
_exptl_absorpt_correction_T_max  0.4949
_exptl_absorpt_correction_T_min  0.4157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004-2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.441
_refine_diff_density_min         -2.388
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         15688
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.335
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0071P)^2^+32.2440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                14493
_reflns_number_total             15688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807808d.txt
_cod_data_source_block           complex_4
_cod_database_code               7004478
_audit_block_refno               678