Crystal structure of bis(η^5^-cyclopentadienyl)(1,4-di-<i>tert</i>-butylbuta-1-en-3-yn-1-yl)zirconium(IV) μ~2~-hydroxido-bis[tris(pentafluorophenyl)borate]
Burlakov, Vladimir V.; Spannenberg, Anke; Arndt, Perdita; Rosenthal, Uwe; Acta Crystallographica Section E 71 (2015) m71–m72; doi:10.1107/S2056989015003710

data_2240465
_publ_section_title
;
 Crystal structure of
 bis(\h^5^-cyclopentadienyl)(1,4-di-<i>tert</i>-butylbuta-1-en-3-yn-1-yl)zirconium(IV)
 \m~2~-hydroxido-bis[tris(pentafluorophenyl)borate]
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m71
_journal_page_last               m72
_journal_paper_doi               10.1107/S2056989015003710
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Zr (C12 H19) (C5 H5)2] (C36 H B2 F30 O)'
_chemical_formula_moiety         'C22 H29 Zr +, C36 H B2 F30 O -'
_chemical_formula_sum            'C58 H30 B2 F30 O Zr'
_chemical_formula_weight         1425.66
_chemical_name_systematic
'Bis(\h^5^-cyclopentadienyl)(1,4-di-<i>tert</i>-butylbuta-1-en-3-yn-1-yl)zirconium(IV) \m~2~-hydroxido-bis[tris(pentafluorophenyl)borate]'
_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   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                86.730(3)
_cell_angle_beta                 75.389(3)
_cell_angle_gamma                77.581(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8896(5)
_cell_length_b                   13.6334(5)
_cell_length_c                   16.5466(6)
_cell_measurement_reflns_used    6318
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      1.64
_cell_volume                     2747.84(18)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2005)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2005)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2005)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47172
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.037
_diffrn_reflns_theta_min         1.529
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.8103
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe & Cie, 2005)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       prism
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.405
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         13119
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.848
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0453P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                8407
_reflns_number_total             13119
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nr2057sup1.cf
_cod_data_source_block           I
_cod_database_code               2240465
_cod_database_fobs_code          2240465
_shelx_hkl_checksum              59941
_shelx_res_checksum              53172
_shelxl_version_number           2.014