Bridging N-Aminoisocyanate Ligands in Heterobimetallic Complexes: Coupling of Zirconium Hydrazinediides and Transition-Metal Carbonyls
Gehrmann, Thorsten; Lloret Fillol, Julio; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 29 (2010) 28–; doi:10.1021/om900877c

data_4067345
_publ_section_title
;
 Bridging N-Aminoisocyanate Ligands in Heterobimetallic Complexes:
 Coupling of Zirconium Hydrazinediides and Transition-Metal Carbonyls
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              28
_journal_paper_doi               10.1021/om900877c
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C54.5 H68 Cr N6 O6 Si2 Zr'
_chemical_formula_weight         1102.55
_chemical_properties_physical    air-sensitive
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tg18
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.841(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.239(5)
_cell_length_b                   22.213(12)
_cell_length_c                   22.686(11)
_cell_measurement_reflns_used    7886
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.85
_cell_measurement_theta_min      2.19
_cell_volume                     5657(5)
_computing_cell_refinement
;
SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_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    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'CCD-PXL-KAF2 (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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            143033
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         32.28
_diffrn_reflns_theta_min         0.92
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.536(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1361
_refine_ls_number_reflns         36479
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0413P)^2^+2.8564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                30388
_reflns_number_total             36479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900877c_si_002.cif
_cod_data_source_block           complex_2a
_cod_original_sg_symbol_H-M      'P n'
_cod_original_formula_sum        'C54.50 H68 Cr N6 O6 Si2 Zr'
_cod_database_code               4067345
_audit_block_refno               886