Synthesis and Properties of Boranocarbonate: A Convenient in Situ CO Source for the Aqueous Preparation of [99mTc(OH2)3(CO)3]+
Roger Alberto; Kirstin Ortner; Nigel Wheatley; Roger Schibli; August P. Schubiger; Journal of the American Chemical Society 123 (2001) 3135–3136; doi:10.1021/ja003932b

data_4115468
_publ_contact_author_address
'Institute of Inorganic Chemistry, University of Zuerich, CH-8057 Zuerich'
_publ_contact_author_email       ariel@aci.unizh.ch
_publ_contact_author_fax         +41-1-6356803
_publ_contact_author_name        'Roger Alberto'
_publ_contact_author_phone       +41-1-6364631
_publ_section_title
;
 Synthesis and Properties of Boranocarbonate: A Convenient in Situ CO
 Source for the Aqueous Preparation of [99mTc(OH2)3(CO)3]+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3135
_journal_page_last               3136
_journal_paper_doi               10.1021/ja003932b
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         'CH3 B O2H, C18 H36 K N2 O6'
_chemical_formula_sum            'C19 H40 B K N2 O8'
_chemical_formula_weight         474.44
_chemical_name_common            '[K(cryptand)]H3BCO2H'
_chemical_name_systematic
;
Potassium (4,7,13,16,21,24-hexaoxa-1,10-diazobicyclo[8.8.8]hexacosane)
boranocarbonate
;
_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-97
_cell_angle_alpha                106.269(12)
_cell_angle_beta                 105.153(12)
_cell_angle_gamma                111.573(11)
_cell_formula_units_Z            2
_cell_length_a                   11.1315(11)
_cell_length_b                   11.4183(11)
_cell_length_c                   12.4438(13)
_cell_measurement_reflns_used    196
_cell_measurement_temperature    183(2)
_cell_volume                     1289.0(3)
_computing_cell_refinement       'IPDS (STOE, 1999)'
_computing_data_collection       'IPDS (STOE, 1999)'
_computing_data_reduction        'X-RED (STOE, 1999)'
_computing_molecular_graphics    'Zortep (Zsolnai, 1994), Platon (Spek, 1993)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       '/f oscillation 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    0.0893
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5782
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  7.7
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.9520
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.821
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                3003
_reflns_number_total             5782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja003932b.cif
_cod_data_source_block           JA003932B
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] 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^)+(0.0520P)^2^+0.0000P] 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        1289.0(2)
_cod_database_code               4115468