Crystal structure of a zwitterionic azaallyl zirconiumamide complex bearing a Zr^+^-μ-CH~3~—B^{-^} moiety and one equivalent of <i>n</i>-hexane as a solvent
Frerichs, Nils; Adler, Christian; Schmidtmann, Marc; Beckhaus, Rüdiger; IUCrData 3 (2018) x180644–; doi:10.1107/S2414314618006442

data_1549439
_publ_section_title
;
 Crystal structure of a zwitterionic azaallyl zirconiumamide complex
 bearing a Zr^+^-\m-CH~3~---B^{-^} moiety and one equivalent of
 <i>n</i>-hexane as a solvent
;
_journal_coeditor_code           WM4076
_journal_issue                   5
_journal_name_full               IUCrData
_journal_page_first              x180644
_journal_paper_doi               10.1107/S2414314618006442
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac
'[Zr (C19 F18 B1) (C12 H22 N1)2 (C12 H20 N1)], C6 H14'
_chemical_formula_moiety         'C55 H67 B F15 N3 Zr, C6 H14'
_chemical_formula_structural
'[Zr(N(C6H11)2)2(N(C6H11)(C6H9))][BCH3(C6F5)3] C6H14'
_chemical_formula_sum            'C61 H81 B F15 N3 Zr'
_chemical_formula_weight         1243.31
_chemical_name_systematic
'[(Cyclohex-1-enyl)cyclohexylamido]bis(dicyclohexylamido)[methyltris(pentafluorophenyl)borato]zirconium(IV) hexane monosolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.2591(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4930(15)
_cell_length_b                   11.9942(8)
_cell_length_c                   21.8489(14)
_cell_measurement_reflns_used    9306
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.56
_cell_measurement_theta_min      2.24
_cell_volume                     5966.9(7)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            345389
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.971
_diffrn_reflns_theta_min         1.789
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.518
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         26205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                21238
_reflns_number_total             26205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4076sup1.cif
_cod_data_source_block           I
_cod_database_code               1549439
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.973
_shelx_hkl_checksum              11036
_shelx_res_checksum              24472
_cod_database_fobs_code 1549439