Zirconium Chelates of a Bulky Ferrocene-Based Diamido Ligand
Siemeling, Ulrich; Auch, Tanja-Corinna; Tomm, Sabine; Fink, Heinrich; Bruhn, Clemens; Neumann, Beate; Stammler, Hans-Georg; Organometallics 26 (2007) 1112–; doi:10.1021/om061063e

data_4072814
_publ_section_title
;
 Zirconium Chelates of a Bulky Ferrocene-Based Diamido Ligand
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1112
_journal_paper_doi               10.1021/om061063e
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         '2(C54 H68 Fe N2 Zr), C7 H7'
_chemical_formula_sum            'C115 H143 Fe2 N4 Zr2'
_chemical_formula_weight         1875.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                104.515(5)
_cell_angle_beta                 102.502(5)
_cell_angle_gamma                95.830(6)
_cell_formula_units_Z            1
_cell_length_a                   12.2718(9)
_cell_length_b                   14.0496(10)
_cell_length_c                   15.2858(10)
_cell_measurement_reflns_used    41014
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      1.42
_cell_volume                     2456.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      ' 360 frames, detector distance = 135 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31993
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.42
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.50
_diffrn_source_voltage           50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.9346
_exptl_absorpt_correction_T_min  0.7619
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-red ver. 1.06 (Stoe & Cie. 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             993
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.708
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0052(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         8579
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                7166
_reflns_number_total             8579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061063esi20061120_120547.cif
_cod_data_source_block           i0117
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072814