Coordination and Reactivity Study of Titanium and Zirconium Complexes of the First Imidazol-2-imine Ethenolate Ligand
Larocque, Timothy G.; Dastgir, Sarim; Lavoie, Gino G.; Organometallics 32 (2013) 4314–; doi:10.1021/om4004708

data_4081141
_publ_section_title
;
 Coordination and Reactivity Study of Titanium and Zirconium Complexes of
 the First Imidazol-2-imine Ethenolate Ligand
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4314
_journal_paper_doi               10.1021/om4004708
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         '2(C34 H34 Cl3 N3 O Zr), C4 H10 O'
_chemical_formula_sum            'C36 H39 Cl3 N3 O1.5 Zr'
_chemical_formula_weight         735.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.002(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.5416(5)
_cell_length_b                   15.8284(6)
_cell_length_c                   27.0557(8)
_cell_measurement_reflns_used    60949
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     7082.8(4)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'CAMERON (Watkin, Prout & Pearce, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0728
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            59156
_diffrn_reflns_theta_full        27.03
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         15425
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+24.0849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                9883
_reflns_number_total             15425
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4004708_si_002.cif
_cod_data_source_block           k11228
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4081141