Zirconium and hafnium complexes supported by linked bis(β-diketiminate) ligands: synthesis, characterization and catalytic application in ethylene polymerization
Gong, Shaogang; Ma, Haiyan; Huang, Jiling; Dalton Transactions  (2009) 8237–8247; doi:10.1039/b905392a

data_7002422
_publ_section_title
;
 Zirconium and hafnium complexes supported by linked
 bis(\b-diketiminate) ligands: synthesis, characterization and
 catalytic application in ethylene polymerization
;
_journal_issue                   39
_journal_name_full               'Dalton Transactions'
_journal_page_first              8237
_journal_page_last               8247
_journal_paper_doi               10.1039/b905392a
_journal_year                    2009
_chemical_formula_sum            'C39.5 H56 Cl2 N4 Zr'
_chemical_formula_weight         749.00
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.609(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4820(11)
_cell_length_b                   31.485(3)
_cell_length_c                   11.7046(11)
_cell_measurement_reflns_used    1850
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.730
_cell_measurement_theta_min      4.550
_cell_volume                     3934.0(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22563
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75156
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.419
_exptl_crystal_size_min          0.347
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.00053(17)
_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   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         8553
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                6286
_reflns_number_total             8553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b905392a.txt
_cod_data_source_block           cd27456
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3933.9(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C39.50 H56 Cl2 N4 Zr'
_cod_database_code               7002422