Preparation and structural studies of neutral oxorhenium(V) complexes with D-penicillamine methyl ester
Kirsch, Sylvia; Noll, Bernhard; Spies, Hartmut; Leibnitz, Peter; Scheller, Dieter; Krueger, Torsten; Johannsen, Bernd; Journal of the Chemical Society, Dalton Transactions  (1998) 455–; doi:10.1039/a706127g

data_7028106
_publ_section_title
;
 Preparation and structural studies of neutral oxorhenium(V) complexes
 with D-penicillamine methyl ester
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              455
_journal_paper_doi               10.1039/a706127g
_journal_year                    1998
_chemical_formula_sum            'C10 H19 N2 O5 Re S2'
_chemical_formula_weight         497.59
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.930(4)
_cell_length_b                   11.709(4)
_cell_length_c                   21.750(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.44
_cell_measurement_theta_min      8.2
_cell_volume                     1510.2(12)
_computing_cell_refinement       CAD4-MOLEN
_computing_data_collection       CAD4-MOLEN
_computing_data_reduction        CAD4-MOLEN-PROCESS
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'ENRAF-NONIUS CAD4'
_diffrn_measurement_method       'omega/2teta scan variable'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            3956
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        1.9
_diffrn_standards_interval_count 180
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    8.342
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.189
_exptl_crystal_description       'transparent blocks'
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.652
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(14)
_refine_ls_extinction_coef       0.0024(2)
_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_all   1.131
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_obs          0.0299
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+16.5600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0768
_refine_ls_wR_factor_obs         0.0754
_reflns_number_observed          3319
_reflns_number_total             3420
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            g706127sup1.cif
_cod_data_source_block           re37d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+16.5600P] 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^)+(0.0203P)^2^+16.5600P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1510.1(12)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7028106