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_1550509
_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_moiety         'C24 H34 Si Zr'
_chemical_formula_sum            'C24 H34 Si Zr'
_chemical_formula_weight         441.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   52.1310(14)
_cell_length_b                   19.3460(5)
_cell_length_c                   8.7251(3)
_cell_measurement_reflns_used    23732
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.1530
_cell_measurement_theta_min      4.8480
_cell_volume                     8799.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.01(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0365
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            42887
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.493
_diffrn_reflns_theta_min         4.877
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.628
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       shard
_exptl_crystal_F_000             3712
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
The Flack x parameter was refined by means of TWIN and BASF to yield -0.022(9).
Within 3 standard deviations, this value is 0 and so indicates a valid
absolute structure determination.
The Hooft parameter was calculated using Platon to be -0.025(1).
The Bayesian statistics based on the Bijvoet pair analysis indicate that the 
correct absolute structure has been assigned with a probability of 100%. 
;
_refine_ls_abs_structure_Flack   -0.022(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4497
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0269P)^2^+8.7062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0421
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4471
_reflns_number_total             4497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01796d2.cif
_cod_data_source_block           072ZRT18
_cod_depositor_comments
'Adding full bibliography for 1550506--1550510.cif.'
_cod_database_code               1550509
_shelx_estimated_absorpt_t_min   0.409
_shelx_estimated_absorpt_t_max   0.833
_oxdiff_exptl_absorpt_empirical_full_min 0.820
_oxdiff_exptl_absorpt_empirical_full_max 1.322
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_refine_ls_abs_structure_hooft   -0.025(1)
_shelxl_version_number           2014-3
_shelx_res_checksum              37266