pH-Controlled Coordination Mode Rearrangements of "Clickable" Huisgen-Based Multidentate Ligands with [MI(CO)3]+ (M = Re,99mTc)
Shalina C. Bottorff; Adam L. Moore; Ariana R. Wemple; Dejan-Krešimir Bučar; Leonard R. MacGillivray; Paul D. Benny; Inorganic Chemistry 52 (2013) 2939–2950; doi:10.1021/ic302330u

data_4334116
_publ_contact_author_address
;
Department of Chemistry,
Washington State University, 
PO Box 644630, 
Pullman, WA 99164, USA 
;
_publ_contact_author_email       bennyp@wsu.edu
_publ_contact_author_name        'Bennny, Paul D.'
_publ_contact_author_phone       509-335-3858
_publ_section_title
;
 pH-Controlled Coordination Mode Rearrangements of "Clickable"
 Huisgen-Based Multidentate Ligands with [MI(CO)3]+ (M = Re,99mTc)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2939
_journal_page_last               2950
_journal_paper_doi               10.1021/ic302330u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C22 H21 N5 O5 Re, C F3 O3 S'
_chemical_formula_sum            'C23 H21 F3 N5 O8 Re S'
_chemical_formula_weight         770.71
_chemical_name_systematic
;
 ?
;
_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_date             2011-01-04T00:31:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.232(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8352(16)
_cell_length_b                   14.5582(16)
_cell_length_c                   12.6615(14)
_cell_measurement_reflns_used    12249
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.00
_cell_volume                     2662.0(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo, Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Mercury (Macrae, 2008)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.038
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17505
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    4.722
_exptl_absorpt_correction_T_max  0.8156
_exptl_absorpt_correction_T_min  0.4098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_description       bar
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.859
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                3675
_reflns_number_total             4682
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302330u_si_002_3.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334116