Conformationally dynamic titanium and zirconium cationic complexes of bis(naphthoxy)pyridine ligands: structure, "oscillation" and olefin polymerization catalysis.
Annunziata, Liana; Roisnel, Thierry; Razavi, Abbas; Carpentier, Jean-François; Kirillov, Evgueni; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3150–3159; doi:10.1039/c6dt04680k

data_7041900
_publ_section_title
;
 Conformationally dynamic titanium and zirconium cationic complexes of
 bis(naphthoxy)pyridine ligands: structure, &quot;oscillation&quot; and
 olefin polymerization catalysis.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3150
_journal_page_last               3159
_journal_paper_doi               10.1039/c6dt04680k
_journal_volume                  46
_journal_year                    2017
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C39 H50 Cl2 N2 O2 Si2 Zr, 7/3(C6 H6)'
_chemical_formula_sum            'C53 H64 Cl2 N2 O2 Si2 Zr'
_chemical_formula_weight         979.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-11-29T09:41:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-12-11 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                69.667(2)
_cell_angle_beta                 75.579(2)
_cell_angle_gamma                70.528(2)
_cell_formula_units_Z            6
_cell_length_a                   18.8689(10)
_cell_length_b                   20.4867(11)
_cell_length_c                   22.9343(13)
_cell_measurement_reflns_used    9069
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.93
_cell_measurement_theta_min      2.38
_cell_measurement_wavelength     0.71073
_cell_volume                     7748.1(7)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 1999),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.961
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            116649
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.851
_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    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3084
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.259
_refine_diff_density_min         -2.184
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1459
_refine_ls_number_reflns         34197
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+14.9282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                23205
_reflns_number_total             34197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt04680k2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
Adding full bibliography for 7041899--7041900.cif.

2017-11-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C159 H192 Cl6 N6 O6 Si6 Zr3'
_cod_original_formula_weight         2938.09
_cod_original_formula_moiety         '3(C39 H50 Cl2 N2 O2 Si2 Zr), 7(C6 H6)'
_cod_original_formula_units_Z            2
_cod_database_code               7041900