Group 4 permethylindenyl complexes for slurry-phase polymerisation of ethylene
Lamb, Jessica V.; Buffet, Jean-Charles; Turner, Zoë R.; O'Hare, Dermot; Polymer Chemistry 10 (2019) 1386–; doi:10.1039/C8PY01796D

data_1550508
_publ_section_title
;
 Group 4 permethylindenyl complexes for slurry-phase polymerisation of
 ethylene
;
_journal_issue                   11
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1386
_journal_paper_doi               10.1039/C8PY01796D
_journal_volume                  10
_journal_year                    2019
_chemical_formula_sum            'C26 H36 Cl2 Si Zr'
_chemical_formula_weight         538.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-12-06 deposited with the CCDC.
2019-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                104.583(2)
_cell_angle_beta                 94.052(2)
_cell_angle_gamma                103.622(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7586(2)
_cell_length_b                   11.3702(3)
_cell_length_c                   14.6917(4)
_cell_measurement_reflns_used    14168
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.1890
_cell_measurement_theta_min      4.1000
_cell_volume                     1362.94(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
ORTEP3 for Windows. Farrugia, L. J. J. Appl. Cryst. 1997, 30, 565.
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution
;
SUPERFLIP 
Palatinus, L.; Chapuis, G. J. Appl. Cryst. 2007, 40, 786-790.
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27786
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.498
_diffrn_reflns_theta_min         4.163
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
TITL 009ZRT17 in P-1
CELL    8.7586   11.3702   14.6917    104.58     94.05    103.62
SPGR P-1
C101 0.018 0.468 0.004 !       4.47 eA-3
C102 0.905 0.619 0.156 !       3.84 eA-3
C103 0.941 0.564 0.046 !       3.61 eA-3
C104 0.955 0.535 0.097 !       3.61 eA-3
Q105 0.082 1.004 0.205 !       1.38 eA-3
Q106 0.109 0.328 0.200 !       1.21 eA-3
Q107 0.614 0.408 0.332 !       0.95 eA-3
C108 0.139 0.495 0.031 !       0.76 eA-3
C109 0.029 0.622 0.019 !       0.68 eA-3
C110 0.883 0.449 0.115 !       0.58 eA-3
C111 0.966 0.727 0.139 !       0.50 eA-3
;
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0284P)^2^+0.5663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5170
_reflns_number_total             5566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01796d2.cif
_cod_data_source_block           009ZRT17
_cod_depositor_comments
'Adding full bibliography for 1550506--1550510.cif.'
_cod_database_code               1550508
_shelx_estimated_absorpt_t_min   0.303
_shelx_estimated_absorpt_t_max   0.850
_shelxl_version_number           2014-3
_shelx_res_checksum              41868
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              89366