In Vitro Anticancer Activity and in Vivo Biodistribution of Rhenium(I) Tricarbonyl Aqua Complexes
Knopf, Kevin M.; Murphy, Brendan L.; MacMillan, Samantha N.; Baskin, Jeremy M.; Barr, Martin P.; Boros, Eszter; Wilson, Justin J.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08640

data_4126483
_publ_section_title
;
 In Vitro Anticancer Activity and in Vivo Biodistribution of Rhenium(I)
 Tricarbonyl Aqua Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08640
_journal_year                    2017
_chemical_formula_moiety         'C17 H15 N3 O5 Re, 0.93(B F4), 0.07(Cl)'
_chemical_formula_sum            'C17 H15 B0.93 Cl0.07 F3.73 N3 O5 Re'
_chemical_formula_weight         610.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.033(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9967(7)
_cell_length_b                   17.2578(12)
_cell_length_c                   12.1669(9)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.90
_cell_volume                     2083.3(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      223.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22605
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.368
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.908
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0786 before and 0.0414 after correction. 
The Ratio of minimum to maximum transmission is 0.7839. 
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_description       Block
_exptl_crystal_F_000             1169
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0202
_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^)+(0.0181P)^2^+1.1330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4688
_reflns_number_total             5369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08640_si_002.cif
_cod_data_source_block           10_BF4
_cod_database_code               4126483
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.514
_shelx_estimated_absorpt_t_min   0.270
_exptl_absorpt_special_details   none
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{B, Cl}
3. Uiso/Uaniso restraints and constraints
Uanis(B) = Uanis(Cl)
4. Others
 Sof(Cl)=1-FVAR(1)
 Sof(B)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C10(H10), C12(H12), C13(H13)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              74069
_shelx_hkl_checksum              8070
_olex2_submission_special_instructions 'No special instructions were received'