Synthesis, Characterization, and Thermal Rearrangement of Zirconium Tetraazadienyl and Pentaazadienyl Complexes
Gehrmann, Thorsten; Lloret Fillol, Julio; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 31 (2012) 4504–; doi:10.1021/om300291b

data_4078520
_publ_section_title
;
 Synthesis, Characterization, and Thermal Rearrangement of Zirconium
 Tetraazadienyl and Pentaazadienyl Complexes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              4504
_journal_paper_doi               10.1021/om300291b
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C50 H76 N8 Si3 Zr'
_chemical_formula_weight         964.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tg9
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.037(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0891(10)
_cell_length_b                   24.999(2)
_cell_length_c                   16.8649(14)
_cell_measurement_temperature    100(2)
_cell_volume                     5058.4(7)
_computing_cell_refinement       'SAINT (Bruker AXS, 1997-2008)'
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2008)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD (Sheldrick, 2000-4)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            85154
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6786
_exptl_absorpt_correction_type   'multi-scan (Blessing, 1995)'
_exptl_absorpt_process_details   'SADABS (Sheldrick & Bruker AXS, 2004-2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.064
_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   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         8898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0442P)^2^+5.2960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                7469
_reflns_number_total             8898
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300291b_si_002.cif
_cod_data_source_block           complex_10
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4078520
_audit_block_refno               772