Methyltriskaidecazirconates, Molecular Forms of Zirconia
Victor W. Day; Walter G. Klemperer; Margaret Mary Pafford; Inorganic Chemistry 44 (2005) 5397–5404; doi:10.1021/ic048307c

data_4309242
_publ_contact_author_address
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Department of Chemistry 
University of Illinois
600 South Mathews Avenue
Urbana, IL 61801
U.S.A.
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_publ_contact_author_email       wklemper@uiuc.edu
_publ_contact_author_fax         '217 333 2685'
_publ_contact_author_name        'Walter G. Klemperer'
_publ_contact_author_phone       '217 333 2995'
_publ_section_title
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Methyltriskaidecazirconates, Molecular Forms of Zirconia
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5397
_journal_page_last               5404
_journal_paper_doi               10.1021/ic048307c
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C33 H96 O44 Zr13'
_chemical_formula_weight         2382.96
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           160
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   17.2672(6)
_cell_length_b                   17.2672(6)
_cell_length_c                   27.4602(19)
_cell_measurement_reflns_used    1533
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.269
_cell_measurement_theta_min      2.225
_cell_volume                     7090.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1128
_diffrn_reflns_av_sigmaI/netI    0.1254
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            14755
_diffrn_reflns_theta_full        26.72
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'near cube'
_exptl_crystal_F_000             3498
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(19)
_refine_ls_extinction_coef       0.000045(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         3641
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0610P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                1612
_reflns_number_total             3641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048307csi20041130_050459.cif
_cod_data_source_block           wks3#160
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4309242