Oxorhenium(V) and Oxotechnetium(V) Complexes of Cysteine
Mita Chatterjee; Basudeb Achari; Satyabrata Das; Rahul Banerjee; Chandana Chakrabarti; Jiban K. Dattagupta; Somenath Banerjee; Inorganic Chemistry 37 (1998) 5424–5430; doi:10.1021/ic970577q

data_4323089
_publ_section_title
;
 Oxorhenium(V) and Oxotechnetium(V) Complexes of Cysteine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5424
_journal_page_last               5430
_journal_paper_doi               10.1021/ic970577q
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source
;
 Compound has been synthesised, purified and
 crystallized in the laboratory. 
;
_chemical_formula_moiety
;
 Re O (C6 H11 N2 O4 S2),Re O (C6 H10 N2 O4 S2) 1-
,P(C6 H5)4 1+,4(H2 O)
;
_chemical_formula_sum            'C36 H49 N4 O14 P Re2 S4'
_chemical_formula_weight         1293.40
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.700(2)
_cell_length_b                   12.836(3)
_cell_length_c                   36.228(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      9
_cell_volume                     4510.7(15)
_computing_cell_refinement       ' CAD-4 software (Enraf Nonius,1989) '
_computing_data_collection       ' CAD-4 software (Enraf Nonius,1989) '
_computing_data_reduction        'SDP (Enraf Nonius,1985) '
_computing_molecular_graphics    ' ORTEX 2.1a (McArdle, 1993)'
_computing_publication_material  ' SHELXL-93 (Sheldrick, 1993) '
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 diffractometer '
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5186
_diffrn_reflns_theta_max         74.93
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        'not significant'
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.980
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.6559
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_meas      1.94(2)
_exptl_crystal_density_method    'flotation in benzene-bromoform mixture'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             2500
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         5.146
_refine_diff_density_min         -3.202
_refine_diff_density_rms         0.230
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.00043(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.775
_refine_ls_goodness_of_fit_obs   0.782
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         5184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.775
_refine_ls_restrained_S_obs      0.782
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_obs          0.0638
_refine_ls_shift/esd_max         -8.354
_refine_ls_shift/esd_mean        0.520
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1410P)^2^+90.1287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1694
_refine_ls_wR_factor_obs         0.1679
_reflns_number_observed          5016
_reflns_number_total             5184
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970577q.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1410P)^2^+90.1287P] 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^)+( 0.1410P)^2^+90.1287P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323089