Syntheses and structures of zirconium(IV) complexes supported by 2,6-di-adamantylaryloxide ligands and formation of arene-bridged dizirconium complexes with an inverse sandwich structure.
Watanabe, Takahito; Ishida, Yutaka; Matsuo, Tsukasa; Kawaguchi, Hiroyuki; Dalton transactions (Cambridge, England : 2003) 39 (2010) 484–491; doi:10.1039/b911082h

data_7024102
_publ_section_title
;
 Syntheses and structures of zirconium(IV) complexes supported by
 2,6-di-adamantylaryloxide ligands and formation of arene-bridged
 dizirconium complexes with an inverse sandwich structure.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              484
_journal_page_last               491
_journal_paper_doi               10.1039/b911082h
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C54 H70 Cl2 O2 Zr, 0.5(C6 H14)'
_chemical_formula_sum            'C57 H77 Cl2 O2 Zr'
_chemical_formula_weight         956.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.960(2)
_cell_length_b                   19.240(4)
_cell_length_c                   41.699(8)
_cell_measurement_reflns_used    23673
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0863
_cell_volume                     9595(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            71788
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.9483
_exptl_absorpt_correction_T_min  0.9070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4072
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.465
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         10746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.465
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+16.7161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                10412
_reflns_number_total             10746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911082h.txt
_cod_data_source_block           ZrCl2[OAr(Me)]2
_cod_original_cell_volume        9596(3)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7024102