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_4320844
_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            'C54 H74 Li2 N4 S6 Zr'
_chemical_formula_weight         1076.70
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source           International_Tables_for_Xray_Crystallography
_cell_angle_alpha                89.93(1)
_cell_angle_beta                 108.00(2)
_cell_angle_gamma                94.42(1)
_cell_formula_units_Z            2
_cell_length_a                   12.606(2)
_cell_length_b                   15.233(2)
_cell_length_c                   16.003(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(1)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     2913.1(10)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_computing_molecular_graphics    ORTEP_(Johnson,_1976)
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  LSFM_MolEN_(Fair,_1990)
_computing_structure_solution    Direct_methods_(MULTAN,_Main_et_al.,_1980)
_diffrn_ambient_temperature      213(1)
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11659
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.34
_diffrn_standards_decay_%        3.65
_diffrn_standards_interval_time  50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.9988
_exptl_absorpt_correction_T_min  0.9400
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.23
_exptl_crystal_description       chunky
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.07
_refine_ls_abs_structure_details
;
?
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.651
_refine_ls_hydrogen_treatment    H_atoms_riding_U=1.3_x_U_bonding_atom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8801
_refine_ls_number_restraints     328
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_obs          0.036
_refine_ls_shift/esd_max         0.009
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.049
_reflns_number_observed          8801
_reflns_number_total             11179
_reflns_observed_criterion       >3.0\s(I)
_cod_data_source_file            ic991402e_1.cif
_cod_data_source_block           '[Li(tmeda)]2[Zr(SC6H4-4-Me)6]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w = 4Fo^2^/
(\s^2^(Fo^2^) + 0.0016 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2913(2)
_cod_original_formula_sum        'C54 H74 Li2 N4 S6 Zr1'
_cod_database_code               4320844