Synthesis and crystallographic characterization of [2,2-bis(η^5^-pentamethylcyclopentadienyl)-3,4-bis(trimethylsilyl)-2-zirconafuran-5-one-κ<i>O</i>^5^]triisobutylaluminium
Burlakov, Vladimir V.; Bogdanov, Vyacheslav S.; Arndt, Perdita; Spannenberg, Anke; Rosenthal, Uwe; Beweries, Torsten; Shur, Vladimir B.; Acta Crystallographica Section E 74 (2018) 566–568; doi:10.1107/S2056989018004759

data_2243634
_publ_section_title
;
 Synthesis and crystallographic characterization of
 [2,2-bis(\h^5^-pentamethylcyclopentadienyl)-3,4-bis(trimethylsilyl)-2-zirconafuran-5-one-\k<i>O</i>^5^]triisobutylaluminium
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              566
_journal_page_last               568
_journal_paper_doi               10.1107/S2056989018004759
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Al Zr (C10 H15)2 (C4 H9)3 (C9 H18 O2 Si2)]'
_chemical_formula_moiety         'C41 H75 Al O2 Si2 Zr'
_chemical_formula_sum            'C41 H75 Al O2 Si2 Zr'
_chemical_formula_weight         774.39
_chemical_name_systematic
'[2,2-Bis(\h^5^-pentamethylcyclopentadienyl)-3,4-bis(trimethylsilyl)-2-zirconafuran-5-one-\k<i>O</i>^5^]triisobutylaluminium'
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.0206(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5404(2)
_cell_length_b                   16.5073(3)
_cell_length_c                   22.9519(4)
_cell_measurement_reflns_used    9039
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.28
_cell_volume                     4355.58(13)
_computing_cell_refinement
;
SAINT (Bruker, 2011)
;
_computing_data_collection
;
APEX2 (Bruker, 2011)
;
_computing_data_reduction
;
SAINT (Bruker, 2011)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            97067
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.522
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2011)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.531
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         10803
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+2.1095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                9409
_reflns_number_total             10803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cq2023sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243634
_shelx_hkl_checksum              90886
_shelx_res_checksum              80042
_cod_database_fobs_code 2243634