Microwave-Assisted Synthesis of 3,1,2- and 2,1,8-Re(I) and99mTc(I)−Metallocarborane Complexes
Green, Andrew E. C.; Causey, Patrick W.; Louie, Anika S.; Armstrong, Andrea F.; Harrington, Laura E.; Valliant, John F.; Inorganic Chemistry 45 (2006) 5727–5729; doi:10.1021/ic0605928

data_4332631
_publ_section_title
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 Microwave-Assisted Synthesis of 3,1,2- and 2,1,8-Re(I)
 and99mTc(I)&#x2212;Metallocarborane Complexes
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_journal_issue                   15
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5727
_journal_page_last               5729
_journal_paper_doi               10.1021/ic0605928
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C12 H17 B9 Na O8 Re'
_chemical_formula_weight         595.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 94.935(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7890(5)
_cell_length_b                   24.5236(9)
_cell_length_c                   7.1903(3)
_cell_measurement_reflns_used    9434
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      35.82
_cell_measurement_theta_min      2.40
_cell_volume                     2071.07(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            38746
_diffrn_reflns_theta_full        36.55
_diffrn_reflns_theta_max         36.55
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    5.926
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.591
_refine_diff_density_min         -3.343
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.00169(18)
_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   1.551
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         9618
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.566
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                7364
_reflns_number_total             9618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0605928sup1.cif
_cod_data_source_block           Compound5
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4332631