Synthesis and structural characterisation of a boralumoxane capable of activating a zirconocene ethene polymerisation catalyst
Richter, Bodo; Meetsma, Auke; Hessen, Bart; Teuben, Jan H.; Chemical Communications  (2001) 1286–; doi:10.1039/b103670j

data_7125474
_publ_section_title
;
 Synthesis and structural characterisation of a boralumoxane capable of
 activating a zirconocene ethene polymerisation catalyst
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1286
_journal_paper_doi               10.1039/b103670j
_journal_year                    2001
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C64 H104 Al4 B4 O8, 2.5(C6 H6)'
_chemical_formula_sum            'C79 H119 Al4 B4 O8'
_chemical_formula_weight         1347,96
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   direct
_audit_creation_date             '2001-05-23  10:27:12'
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
?
;
_cell_angle_alpha                79.888(1)
_cell_angle_beta                 86.886(1)
_cell_angle_gamma                65.389(1)
_cell_formula_units_Z            2
_cell_length_a                   14.0027(5)
_cell_length_b                   14.2483(5)
_cell_length_c                   22.7478(9)
_cell_measurement_reflns_used    9078
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.33
_cell_volume                     4061.2(3)
_computing_cell_refinement       'SAINT, Bruker Version 6.02A, 2000'
_computing_data_collection       'SMART, Bruker Version 5.168, 2000'
_computing_data_reduction        'XPREP, Bruker Version 5.1/NT, 2000'
_computing_molecular_graphics
;
PLUTO (Meetsma, 2001) 
PLATON (Spek, 1994)
;
_computing_publication_material
;
PLATON (Spek, 1990)
SHELXL (Sheldrick, 1997)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      200(1)
_diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)'
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type
;
Bruker Smart Apex 
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_detector
;
CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38591
_diffrn_reflns_reduction_process
;
Intensity data were corrected for Lorentz and polarization
effects, decay and absorption and reduced to F~o~^2^
using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)

Intensity data were corrected for Lorentz and polarization effects,
scale variation, for absorption and reduced to F~o~^2^
;
_diffrn_reflns_theta_full        29.02
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_correction_T_min  0.9482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         20435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.618
_refine_ls_shift/su_mean         0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+0.5086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1689
_reflns_number_gt                13923
_reflns_number_total             20435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103670j.txt
_cod_data_source_block           c79h119a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7125474