Zirconium arene triple-decker sandwich complexes: Synthesis, electronic structure and bonding
Kilpatrick, Alexander Florian Ross; Green, Jennifer; Turner, Zoe; Buffet, Jean-Charles; O’Hare, Dermot; Chem. Commun.  (2017) –; doi:10.1039/C7CC07083G

data_7120771
_publ_section_title
;
 Zirconium arene triple-decker sandwich complexes: Synthesis, electronic
 structure and bonding
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC07083G
_journal_year                    2017
_chemical_formula_moiety         'C36 H46 Zr2'
_chemical_formula_sum            'C36 H46 Zr2'
_chemical_formula_weight         661.17
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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-2014/7
_audit_update_record
;
2017-09-07 deposited with the CCDC.
2017-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                96.3910(10)
_cell_angle_beta                 109.5610(10)
_cell_angle_gamma                90.0210(10)
_cell_formula_units_Z            4
_cell_length_a                   13.3867(2)
_cell_length_b                   14.8682(2)
_cell_length_c                   16.7564(2)
_cell_measurement_reflns_used    72375
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      5.1
_cell_volume                     3120.59(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP3 for Windows. Farrugia, L. J. J. Appl. Cryst. 1997, 30, 565.
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
;
SUPERFLIP 
Palatinus, L.; Chapuis, G. J. Appl. Cryst. 2007, 40, 786-790.
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25997
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.557
_diffrn_reflns_theta_min         5.101
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.84943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Multi-scan from symmetry-related measurements using
Sortav (Blessing, 1995)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         14243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0452P)^2^+0.4556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10296
_reflns_number_total             14243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07083g2.cif
_cod_data_source_block           Compound4
_cod_database_code               7120771
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.820
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              89971