Unexpected Reactions between Ziegler-Natta Catalyst Components and Structural Characterization of Resulting Intermediates.
Sobota, Piotr; Utko, Józef; Lis, Tadeusz; John, Łukasz; Petrus, Rafał; Drąg-Jarząbek, Anna; Inorganic chemistry 55 (2016) 4636–4642; doi:10.1021/acs.inorgchem.6b00489

data_4347694
_publ_section_title
;
 Unexpected Reactions between Ziegler-Natta Catalyst Components and
 Structural Characterization of Resulting Intermediates.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4636
_journal_page_last               4642
_journal_paper_doi               10.1021/acs.inorgchem.6b00489
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C32 H85 Cl3 Mg4 O19 Ti3, 0.5(C2 H6 O)'
_chemical_formula_sum            'C33 H88 Cl3 Mg4 O19.5 Ti3'
_chemical_formula_weight         1144.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.69(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.172(5)
_cell_length_b                   19.331(5)
_cell_length_c                   29.658(6)
_cell_measurement_reflns_used    9360
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      27.4981
_cell_measurement_theta_min      2.7292
_cell_volume                     11325(5)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'DIAMOND  (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            30478
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         2.735
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             4856
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         13070
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+27.4732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9264
_reflns_number_total             13070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00489_si_002.cif
_cod_data_source_block           3x3a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C33 H88 Cl3 Mg4 O19.50 Ti3'
_cod_database_code               4347694
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              39571
_shelx_hkl_checksum              85918