Cu-Free 1,3-Dipolar Cycloaddition Click Reactions To Form Isoxazole Linkers in Chelating Ligands for fac-[M(I)(CO)3](+) Centers (M = Re, (99m)Tc).
Bottorff, Shalina C.; Kasten, Benjamin B.; Stojakovic, Jelena; Moore, Adam L.; Macgillivray, Leonard R.; Benny, Paul D.; Inorganic chemistry 53 (2014) 1943–1945; doi:10.1021/ic402825t

data_4337247
_publ_section_title
;
 Cu-Free 1,3-Dipolar Cycloaddition Click Reactions To Form Isoxazole
 Linkers in Chelating Ligands for fac-[M(I)(CO)3](+) Centers (M = Re,
 (99m)Tc).
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1943
_journal_page_last               1945
_journal_paper_doi               10.1021/ic402825t
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C21 H16 N3 O6 Re, C H4 O'
_chemical_formula_sum            'C22 H20 N3 O7 Re'
_chemical_formula_weight         624.61
_chemical_melting_point          ?
_chemical_name_common            fac-[ReI(CO)3(10)]
_chemical_name_systematic
;
fac-triscarbonyl(2-(((3-phenylisoxazol-5-yl)methyl)(pyridin-2-ylmethyl)amino)acetate)rhenium(I)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                117.169(5)
_cell_angle_beta                 101.227(5)
_cell_angle_gamma                97.439(5)
_cell_formula_units_Z            2
_cell_length_a                   8.1342(8)
_cell_length_b                   12.5836(13)
_cell_length_c                   12.8618(13)
_cell_measurement_reflns_used    4701
_cell_measurement_temperature    190
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.00
_cell_volume                     1112.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9749
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    5.512
_exptl_absorpt_correction_T_max  0.718
_exptl_absorpt_correction_T_min  0.316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.160
_refine_diff_density_min         -1.992
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5274
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0241P)^2^+2.9097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                4562
_reflns_number_total             5274
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic402825t_si_002.cif
_cod_data_source_block           mcg1370
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1112.28(19)
_cod_database_code               4337247