Highly Thermally Stable Eight-Coordinate Dichloride Zirconium Complexes Supported by Tridentate [ONN] Ligands: Syntheses, Characterization, and Ethylene Polymerization Behavior
Li, Aike; Ma, Haiyan; Huang, Jiling; Organometallics 32 (2013) 7460–; doi:10.1021/om4009636

data_4082163
_publ_section_title
;
 Highly Thermally Stable Eight-Coordinate Dichloride Zirconium Complexes
 Supported by Tridentate [ONN] Ligands: Syntheses, Characterization, and
 Ethylene Polymerization Behavior
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7460
_journal_paper_doi               10.1021/om4009636
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C90 H106 Cl2 N4 O7 Zr'
_chemical_formula_weight         1517.91
_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                110.748(2)
_cell_angle_beta                 107.264(2)
_cell_angle_gamma                95.814(2)
_cell_formula_units_Z            2
_cell_length_a                   15.040(2)
_cell_length_b                   16.687(2)
_cell_length_c                   18.150(2)
_cell_measurement_reflns_used    4716
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      52.857
_cell_measurement_theta_min      4.394
_cell_volume                     3957.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      140(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0926
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24732
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  0.9614
_exptl_absorpt_correction_T_min  0.9131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         14555
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+3.1341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.2171
_reflns_number_gt                9947
_reflns_number_total             14555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4009636_si_002.cif
_cod_data_source_block           dm13439
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3957.5(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082163