Synthesis, properties and crystal structures of 6-, 7- and 8-coordinate Zr(iv) and Hf(iv) complexes involving thioether and selenoether ligands
Hart, Richard; Levason, William; Patel, Bhavesh; Reid, Gillian; Journal of the Chemical Society, Dalton Transactions  (2002) 3153–; doi:10.1039/b201080c

data_7702796
_publ_section_title
;
 Synthesis, properties and crystal structures of 6-, 7- and 8-coordinate
 Zr(iv) and Hf(iv) complexes involving thioether and selenoether ligands
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3153
_journal_paper_doi               10.1039/b201080c
_journal_year                    2002
_chemical_formula_moiety         'C8 H20 Cl4 Hf S4 '
_chemical_formula_structural     '[HfCl4{MeS(CH2)2SMe}2]'
_chemical_formula_sum            'C8 H20 Cl4 Hf S4'
_chemical_formula_weight         564.79
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      96
_symmetry_space_group_name_H-M   'P 43 21 2'
_audit_creation_date             2002-02-18
_audit_creation_method           'by teXsan for Windows v1.06'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9760(2)
_cell_length_b                   9.9760(2)
_cell_length_c                   17.4881(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     1740.43(6)
_computing_cell_refinement       'Nonius CCD Diffractometer Control'
_computing_data_collection       'Nonius CCD Diffractometer Control'
_computing_data_reduction
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_publication_material
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_structure_refinement
'teXsan for Windows version 1.06 (MSC, 1997-1999)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      120.0(1)
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius CCD rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.11969
_diffrn_reflns_av_sigmaI/netI    0.097
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5914
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.054
_exptl_absorpt_correction_type   SORTAV
_exptl_crystal_colour            rod
_exptl_crystal_density_diffrn    2.155
_exptl_crystal_density_meas      ?
_exptl_crystal_description       colourless
_exptl_crystal_F_000             1088.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         -4.33_close_to_Hf
_refine_diff_density_min         3.97_close_to_Hf
_refine_ls_abs_structure_details checked
_refine_ls_abs_structure_Flack   -0.0122(0.00121)
_refine_ls_extinction_coef       -
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.868
_refine_ls_goodness_of_fit_ref   2.870
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     73
_refine_ls_number_reflns         898
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.0400
_refine_ls_shift/su_mean         0.0060
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1090
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                898
_reflns_number_total             1112
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b201080c.txt
_cod_data_source_block           '_01bp029'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 43 21 2  '
_cod_original_formula_sum        'C8 H20 Cl4 Hf S4 '
_cod_database_code               7702796