[Re(CO)3]+Complexes ofexo-Functionalized Tridentate “Click” Macrocycles: Synthesis, Stability, Photophysical Properties, Bioconjugation, and Antibacterial Activity
Noor, Asif; Huff, Gregory S.; Kumar, Sreedhar V.; Lewis, James E. M.; Paterson, Brett M.; Schieber, Christine; Donnelly, Paul S.; Brooks, Heather J. L.; Gordon, Keith C.; Moratti, Stephen C.; Crowley, James D.; Organometallics 33 (2014) 7031–; doi:10.1021/om500664v

data_4085468
_publ_section_title
;
 [Re(CO)3]+Complexes ofexo-Functionalized Tridentate &#x201C;Click&#x201D;
 Macrocycles: Synthesis, Stability, Photophysical Properties,
 Bioconjugation, and Antibacterial Activity
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7031
_journal_paper_doi               10.1021/om500664v
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C29 H26 Br N10 O7 Re'
_chemical_formula_weight         892.71
_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-97
_cell_angle_alpha                93.303(3)
_cell_angle_beta                 90.356(3)
_cell_angle_gamma                108.644(4)
_cell_formula_units_Z            4
_cell_length_a                   10.4722(4)
_cell_length_b                   16.0868(8)
_cell_length_c                   23.1434(7)
_cell_measurement_reflns_used    11325
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.2510
_cell_measurement_theta_min      3.2840
_cell_volume                     3686.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31782
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    4.434
_exptl_absorpt_correction_T_max  0.7768
_exptl_absorpt_correction_T_min  0.4708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Void electron count of 58 electrons can be accounted for by four molecules
of water (10 electrons each) and a molecule of methanol (18 electrons) to give
a total electron count of 58.
;
_refine_diff_density_max         2.784
_refine_diff_density_min         -2.246
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         14778
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+10.6512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                10961
_reflns_number_total             14778
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500664v_si_002.cif
_cod_data_source_block           10a-Re
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085468