Titanium and Zirconium Amido Complexes Ligated by 2,2'-Di(3-methylindolyl)methanes: Synthesis, Characterization, and Ethylene Polymerization Activity
Mark R. Mason; Bassam N. Fneich; Kristin Kirschbaum; Inorganic Chemistry 42 (2003) 6592–6594; doi:10.1021/ic0347236

data_4312354
_publ_contact_author
;
     Professor Mark R. Mason
     Department of Chemistry
     University of Toledo
     Toledo
     OH 43606
     USA
;
_publ_contact_author_email       mmason5@uoft02.utoledo.edu
_publ_contact_author_fax         '(419) 530-4033'
_publ_contact_author_phone       '(419) 530-1532'
_publ_section_title
;
 Titanium and Zirconium Amido Complexes Ligated by
 2,2'-Di(3-methylindolyl)methanes: Synthesis, Characterization, and
 Ethylene Polymerization Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6592
_journal_page_last               6594
_journal_paper_doi               10.1021/ic0347236
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C33 H39 Br N4 Ti'
_chemical_formula_weight         619.49
_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   difmap
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.107(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.969(3)
_cell_length_b                   10.417(2)
_cell_length_c                   18.760(4)
_cell_measurement_reflns_used    5815
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      53.477
_cell_measurement_theta_min      4.596
_cell_volume                     2977.8(10)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18699
_diffrn_reflns_theta_full        28.65
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  0.840519
_exptl_absorpt_correction_T_min  0.609421
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         6939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+6.1822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                5048
_reflns_number_total             6939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0347236si20030908_044746_2.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2977.7(10)
_cod_database_code               4312354