Preparation and reactions of rhenium(VII) trioxo hydrogendiolato complexes and rhenium(VI) oxo bis(diolato) complexes
Edwards, Peter G.; Jokela, Jukka; Lehtonen, Ari; Sillanpää, Reijo; Journal of the Chemical Society, Dalton Transactions  (1998) 3287–; doi:10.1039/a803301c

data_7027970
_publ_section_title
;
 Preparation and reactions of rhenium(VII) trioxo hydrogendiolato
 complexes and rhenium(VI) oxo bis(diolato) complexes
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3287
_journal_paper_doi               10.1039/a803301c
_journal_year                    1998
_chemical_formula_moiety         '[ReO(C6H12O2)]'
_chemical_formula_sum            'C12 H24 O5 Re'
_chemical_formula_weight         434.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           102
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4n -2n'
_symmetry_space_group_name_H-M   'P 42 n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.315(2)
_cell_length_b                   10.315(2)
_cell_length_c                   7.2700(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      20.9
_cell_volume                     773.5(2)
_computing_cell_refinement
;
MSC/AFC5S Control Program (Molecular Structure Corporation, 1995)
;
_computing_data_collection
; 
MSC/AFC Control Program (Molecular Structure Corporation, 1995)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation, 1989)
;
_computing_molecular_graphics    'ORTEP-3 for WINDOWS (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            743
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.864
_exptl_absorpt_correction_T_max  0.254
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_type
;
empirical via \y scans (North, Phillips & Mathews, 1968)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             422
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .32
_exptl_crystal_size_min          .24
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_coef       0.0102(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         403
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+2.2700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                295
_reflns_number_total             403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c803301sup1.cif
_cod_data_source_block           '[ReO(pin)2]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+2.2700P] 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^)+(0.0288P)^2^+2.2700P] 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      P42nm
_cod_database_code               7027970