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_4347693
_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         'C30 H81 Cl3 Mg4 O19 Ti3'
_chemical_formula_sum            'C30 H81 Cl3 Mg4 O19 Ti3'
_chemical_formula_weight         1093.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.97(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.248(3)
_cell_length_b                   27.353(6)
_cell_length_c                   15.776(4)
_cell_measurement_reflns_used    14912
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.9983
_cell_measurement_theta_min      2.9728
_cell_volume                     5257(2)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_device_type  'KUMA KM4 CCD \k-geometry diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38539
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.065
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'long fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.821
_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    1.381
_exptl_crystal_description       needle
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         12869
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0663P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8469
_reflns_number_total             12869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00489_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347693
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.816
_shelx_estimated_absorpt_t_max   0.926
_shelx_res_checksum              45606
_shelx_hkl_checksum              47761