Group 4 Metal Complexes of Fluorous (Di)Alkoxide-(Di)Imino Ligands: Synthesis, Structure, Olefin Polymerization Catalysis, and Decomposition Pathways
Marquet, Nicolas; Kirillov, Evgueni; Roisnel, Thierry; Razavi, Abbas; Carpentier, Jean-François; Organometallics 28 (2009) 606–; doi:10.1021/om8009409

data_4083437
_publ_section_title
;
 Group 4 Metal Complexes of Fluorous (Di)Alkoxide-(Di)Imino Ligands:
 Synthesis, Structure, Olefin Polymerization Catalysis, and Decomposition
 Pathways
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              606
_journal_paper_doi               10.1021/om8009409
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H24 F22 N2 O2 Zr'
_chemical_formula_sum            'C38 H24 F22 N2 O2 Zr'
_chemical_formula_weight         1049.81
_chemical_name_systematic
;
 ?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-09-16T15:57:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.105(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1292(5)
_cell_length_b                   19.7931(9)
_cell_length_c                   19.9920(9)
_cell_measurement_reflns_used    8559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.30
_cell_measurement_wavelength     0.71073
_cell_volume                     3919.0(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38575
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+2.8615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                7457
_reflns_number_total             8934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            complex7d_KIR258_100K_APEX_13avr06_archive.cif
_cod_data_source_block           job
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4083437