Construction of C1-symmetric zirconium complexes by the design of new Salan ligands. Coordination chemistry and preliminary polymerisation catalysis studies.
Cohen, Ad; Yeori, Adi; Kopilov, Jacob; Goldberg, Israel; Kol, Moshe; Chemical communications (Cambridge, England)  (2008) 2149–2151; doi:10.1039/b719834e

data_7103107
_publ_section_title
;
 Construction of C1-symmetric zirconium complexes by the design of new
 Salan ligands. Coordination chemistry and preliminary polymerisation
 catalysis studies.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2149
_journal_page_last               2151
_journal_paper_doi               10.1039/b719834e
_journal_year                    2008
_chemical_formula_moiety         '4(C40 H50 Cl2 N2 O2 Zr), 5(C4 H10 O)'
_chemical_formula_sum            'C180 H250 Cl8 N8 O13 Zr4'
_chemical_formula_weight         3382.36
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   28.4938(6)
_cell_length_b                   17.8978(3)
_cell_length_c                   17.8233(3)
_cell_measurement_reflns_used    5528
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.41
_cell_volume                     9089.5(3)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. \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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29291
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3572
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9894
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+1.3115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                7350
_reflns_number_total             9894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b719834e.txt
_cod_data_source_block           mk182j
_cod_original_sg_symbol_H-M      'I ba2'
_cod_database_code               7103107