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_4312356
_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            'C40.5 H51 Br N4 O Zr'
_chemical_formula_weight         780.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.118(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.192(3)
_cell_length_b                   11.756(2)
_cell_length_c                   16.681(3)
_cell_measurement_reflns_used    8505
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      55.697
_cell_measurement_theta_min      5.116
_cell_volume                     3784.3(11)
_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 0.907
_diffrn_measured_fraction_theta_max 0.907
_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  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24523
_diffrn_reflns_theta_full        28.84
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_T_max  0.841234
_exptl_absorpt_correction_T_min  0.604918
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1620
_refine_diff_density_max         1.726
_refine_diff_density_min         -2.421
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         8986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1256P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1858
_reflns_number_gt                6288
_reflns_number_total             8986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0347236si20030908_044746_4.cif
_cod_data_source_block           4b
_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 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3784.2(11)
_cod_original_formula_sum        'C40.50 H51 Br N4 O Zr'
_cod_database_code               4312356