Re and Tc Complexes Containing B-H...M Agostic Interactions as Building Blocks for the Design of Radiopharmaceuticals
Raquel Garcia; António Paulo; Ângela Domingos; Isabel Santos; Kirstin Ortner; Roger Alberto; Journal of the American Chemical Society 122 (2000) 11240–11241; doi:10.1021/ja002652t

data_4116236
_publ_section_title
;
 Re and Tc Complexes Containing B-H...M Agostic Interactions as Building
 Blocks for the Design of Radiopharmaceuticals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11240
_journal_page_last               11241
_journal_paper_doi               10.1021/ja002652t
_journal_volume                  122
_journal_year                    2000
_chemical_formula_structural     '[Tc{H2B(timMe)2}(CO)3](2).0.5CHCl3'
_chemical_formula_sum            'C11.5 H12.5 B Cl1.5 N4 O3 S2 Tc'
_chemical_formula_weight         480.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                83.739(9)
_cell_angle_beta                 82.477(9)
_cell_angle_gamma                87.616(9)
_cell_formula_units_Z            4
_cell_length_a                   7.1363(5)
_cell_length_b                   11.5834(9)
_cell_length_c                   22.942(2)
_cell_measurement_reflns_used    272
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     1868.2(3)
_computing_cell_refinement       'IPDS (STOE, 1999)'
_computing_data_collection       'IPDS (STOE, 1999)'
_computing_data_reduction        'X-RED (STOE, 1999) '
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'STOE IPDS'
_diffrn_measurement_method       '/f oscillatin scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14589
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  6.9
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.9243
_exptl_absorpt_correction_T_min  0.8017
_exptl_absorpt_correction_type   'numerical (Coppens et al, 1965)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.947
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_restrained_S_obs      1.160
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_obs          0.0375
_refine_ls_shift/esd_max         -0.011
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+3.6684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1043
_refine_ls_wR_factor_obs         0.1025
_reflns_number_observed          5669
_reflns_number_total             6691
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja002652t_2.cif
_cod_data_source_block           '[Tc{H2B(timMe)2}(CO)3](2).0.5CHCl3'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+3.6684P] 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^)+(0.0560P)^2^+3.6684P] 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        1868.2(2)
_cod_original_formula_sum        'C11.50 H12.50 B Cl1.50 N4 O3 S2 Tc'
_cod_database_code               4116236