Trigonal Prismatic vs Octahedral Coordination Geometry: Syntheses and Structural Characterization of Hexakis(arylthiolato) Zirconate Complexes
Jan C. Friese; Arndt Krol; Carsten Puke; Kristin Kirschbaum; Dean M. Giolando; Inorganic Chemistry 39 (2000) 1496–1500; doi:10.1021/ic991402e

data_4320845
_publ_contact_author
;
     Prof. Dr. Dean M. Giolando
     Department of Chemistry
     University of Toledo
     Toledo
     OH 43606
     USA
;
_publ_contact_author_email       KKIRSCH@UofT02.UTOLEDO.EDU
_publ_contact_author_fax         '(419) 530-4033'
_publ_contact_author_phone       '(419) 530-4314'
_publ_section_title
;
 Trigonal Prismatic vs Octahedral Coordination Geometry: Syntheses and
 Structural Characterization of Hexakis(arylthiolato) Zirconate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1496
_journal_page_last               1500
_journal_paper_doi               10.1021/ic991402e
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C66 H90 Li2 O12 S6 Zr'
_chemical_formula_weight         1372.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           155
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   'geom except THF-H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.5924(2)
_cell_length_b                   16.5924(2)
_cell_length_c                   21.7663(5)
_cell_measurement_reflns_used    6338
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      13.26
_cell_measurement_theta_min      2.99
_cell_volume                     5189.60(15)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL and the Toledo cifomatic'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measurement_device       Platform
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10356
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.962326
_exptl_absorpt_correction_T_min  0.567892
_exptl_absorpt_correction_type
'Empirical: Multipole Expansion (Blessing,1995)'
_exptl_crystal_colour            'yellow '
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    '?                 '
_exptl_crystal_description       'columnar '
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.09(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.100
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_hydrogen_treatment    'refU except methyl-H noref'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_obs          0.0611
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+4.3733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1689
_refine_ls_wR_factor_obs         0.1579
_reflns_number_observed          1919
_reflns_number_total             2284
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991402e_2.cif
_cod_data_source_block           '[Li(THF)3]2[Zr(SC6H4-4-OMe)6]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+4.3733P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+4.3733P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               4320845