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_4337036
_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_moiety         'C96 H84 O40 Zr12, 4(C3 H7 N O), 4(Cl)'
_chemical_formula_sum            'C108 H112 Cl4 N4 O44 Zr12'
_chemical_formula_weight         3406.45
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.09790(10)
_cell_length_b                   23.09790(10)
_cell_length_c                   16.4166(3)
_cell_measurement_reflns_used    29384
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      75.6750
_cell_measurement_theta_min      3.8100
_cell_volume                     8758.47(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            87533
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.665
_diffrn_reflns_theta_min         3.303
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    6.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79801
_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    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9176
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0653P)^2^+25.1068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7561
_reflns_number_total             9176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402428m_si_003.cif
_cod_data_source_block           Zr-tetrahedron-2
_cod_original_cell_volume        8758.47(18)
_cod_database_code               4337036
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.776