Synthesis, Characterization, and Stereochemistry of Oxorhenium(V) Complexes with 2-Aminoethanethiolate
Takumi Konno; Yuichi Shimazaki; Masayuki Kawai; Masakazu Hirotsu; Inorganic Chemistry 40 (2001) 4250–4256; doi:10.1021/ic010326o

data_4320123
_publ_contact_author
;
Takumi Konno
Department of Chemistry, Graduate School of Science, Osaka 
University, Toyonaka, Osaka 560-0043, Japan
;
_publ_contact_author_email       ' konno@ch.wani.osaka-u.ac.jp'
_publ_contact_author_fax         '+ 81-6-6850-5785'
_publ_contact_author_phone       '+ 81-6-6850-5765'
_publ_section_title
;
 Synthesis, Characterization, and Stereochemistry of Oxorhenium(V)
 Complexes with 2-Aminoethanethiolate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4250
_journal_page_last               4256
_journal_paper_doi               10.1021/ic010326o
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C6 H20 Cl2 N3 O Re S3'
_chemical_formula_weight         503.54
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                102.71(2)
_cell_angle_beta                 101.28(2)
_cell_angle_gamma                75.41(2)
_cell_formula_units_Z            2
_cell_length_a                   11.938(3)
_cell_length_b                   12.366(3)
_cell_length_c                   5.819(1)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    291.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.9
_cell_volume                     802.0(3)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      291.2
_diffrn_measurement_device       'Rigaku AFC7S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.06000
_diffrn_orient_matrix_UB_12      0.04640
_diffrn_orient_matrix_UB_13      0.02054
_diffrn_orient_matrix_UB_21      -0.06371
_diffrn_orient_matrix_UB_22      0.06951
_diffrn_orient_matrix_UB_23      -0.01314
_diffrn_orient_matrix_UB_31      0.00140
_diffrn_orient_matrix_UB_32      0.01521
_diffrn_orient_matrix_UB_33      0.17646
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.010
_diffrn_reflns_av_sigmaI/netI    0.024
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3871
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        -0.19
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.289
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             484.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.38
_refine_diff_density_min         -0.84
_refine_ls_extinction_coef       0.0031(7)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_obs   1.255
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3447
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0207
_refine_ls_shift/esd_max         0.0490
_refine_ls_shift/esd_mean        0.0050
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0272
_reflns_number_observed          3447
_reflns_number_total             3693
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            ic010326o_4.cif
_cod_data_source_block           '[5]Cl2'
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00022|Fo|^2^]' 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) + 0.00022|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C6 H20 Cl2 N3 O S3 Re '
_cod_database_code               4320123