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_7702798
_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_structural     '[Me2SCH2Cl]2[Zr2Cl10]'
_chemical_formula_sum            'C6 H16 Cl12 S2 Zr2'
_chemical_formula_weight         760.19
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2001-12-07
_audit_creation_method           'by teXsan for Windows v1.06'
_cell_angle_alpha                90
_cell_angle_beta                 91.9700(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2646(3)
_cell_length_b                   14.5290(5)
_cell_length_c                   9.3074(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     1252.09(8)
_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      100.0(1)
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       -
_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 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.09997
_diffrn_reflns_av_sigmaI/netI    0.185
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16590
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.269
_exptl_absorpt_correction_type   SORTAV
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_meas      ?
_exptl_crystal_description       colourless
_exptl_crystal_F_000             736.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.95
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_refine_ls_abs_structure_Flack   -
_refine_ls_extinction_coef       -
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.174
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_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         0.0610
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                1349
_reflns_number_total             2659
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b201080c.txt
_cod_data_source_block           '_test'
_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_cell_volume        1252.09(7)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C6 H16 Cl12 S2 Zr2 '
_cod_database_code               7702798