In Situ Construction of a Coordination Zirconocene Tetrahedron
Guoliang Liu; Zhanfeng Ju; Daqiang Yuan; Maochun Hong; Inorganic Chemistry 52 (2013) 13815–13817; doi:10.1021/ic402428m

data_4337038
_publ_section_title
;
 In Situ Construction of a Coordination Zirconocene Tetrahedron
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13815
_journal_page_last               13817
_journal_paper_doi               10.1021/ic402428m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C168 H132 Cl4 O40 Zr12'
_chemical_formula_weight         4027.17
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           216
_space_group_name_Hall           'F -4 2 3'
_space_group_name_H-M_alt        'F -4 3 m'
_symmetry_space_group_name_Hall  'F -4 2 3'
_symmetry_space_group_name_H-M   'F -4 3 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.5532(15)
_cell_length_b                   37.5532(15)
_cell_length_c                   37.5532(15)
_cell_measurement_reflns_used    1768
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      35.5270
_cell_measurement_theta_min      3.8940
_cell_volume                     52959(4)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.702
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.1097
_diffrn_reflns_Laue_measured_fraction_full 0.702
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8272
_diffrn_reflns_point_group_measured_fraction_full 0.701
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         55.691
_diffrn_reflns_theta_min         3.329
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.505
_exptl_crystal_description       block
_exptl_crystal_F_000             8032
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         2449
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      0.822
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1297P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1963
_refine_ls_wR_factor_ref         0.2280
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.699
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                928
_reflns_number_total             2449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402428m_si_005.cif
_cod_data_source_block           Zr-tetrahedron-4
_cod_original_cell_volume        52959(6)
_cod_database_code               4337038
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.936