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_7120773
_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         'C35 H44 Zr2'
_chemical_formula_sum            'C35 H44 Zr2'
_chemical_formula_weight         647.14
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2bc 2ab'
_space_group_name_H-M_alt        'P b n b'
_symmetry_space_group_name_Hall  '-P 2bc 2ab'
_symmetry_space_group_name_H-M   'P b n b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-09-07 deposited with the CCDC.
2017-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1736(5)
_cell_length_b                   14.3455(6)
_cell_length_c                   15.6258(8)
_cell_measurement_reflns_used    3741
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     2953.0(2)
_computing_cell_refinement       'COLLECT (Nonius)'
_computing_data_collection       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    SUPERFLIP
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6359
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_min         5.189
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.84895
_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_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_preparation       'as described'
_exptl_crystal_recrystallization_method
;
toluene solution at ambient temperature
;
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3379
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0430P)^2^+4.8474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1932
_reflns_number_total             3379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07083g2.cif
_cod_data_source_block           Compound2
_cod_database_code               7120773
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.931
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C21, C19, C20, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C21 \\sim C19 \\sim C20 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.03 and
sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C21, C20, C15, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C20(0.5) C15(0.5) H15(0.5)
 C16(0.5) H16(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
6.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id SK-II-08
_olex2_submission_special_instructions 'No special instructions were received'