Rhenium tricarbonyl complexes of AIE active tetraarylethylene ligands: tuning luminescence properties and HSA-specific binding
Gabr, Moustafa T.; Pigge, Chris; Dalton Trans.  (2017) –; doi:10.1039/C7DT03380J

data_7044479
_publ_section_title
;
 Rhenium tricarbonyl complexes of AIE active tetraarylethylene ligands:
 tuning luminescence properties and HSA-specific binding
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03380J
_journal_year                    2017
_chemical_formula_moiety         'C31 H18 Cl N2 O3 Re S2, C7 H8'
_chemical_formula_sum            'C38 H26 Cl N2 O3 Re S2'
_chemical_formula_weight         844.38
_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
_audit_creation_date             2017-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-08-31 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                78.884(5)
_cell_angle_beta                 77.789(5)
_cell_angle_gamma                72.824(5)
_cell_formula_units_Z            2
_cell_length_a                   8.7755(9)
_cell_length_b                   13.4717(14)
_cell_length_c                   15.1412(15)
_cell_measurement_reflns_used    30896
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.6
_cell_volume                     1655.1(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      190.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker-Nonius Kappa ApexII'
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30851
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.653
_diffrn_reflns_theta_min         3.196
_exptl_absorpt_coefficient_mu    3.919
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0742 before and 0.0370 after correction.
The Ratio of minimum to maximum transmission is 0.7682.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         7646
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+1.2158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7097
_reflns_number_total             7646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03380j2.cif
_cod_data_source_block           mg-i(2)
_cod_database_code               7044479
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.341
_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. Restrained distances
 C101-C107 = C111-C117
 1.5 with sigma of 0.02
 C107-C102 \\sim C107-C106 \\sim C117-C112 \\sim C117-C116
 with sigma of 0.01
 C11-C5 \\sim C11'-C5
 with sigma of 0.01
3. Restrained planarity
 C5, C11, S12, C13, C14, C15
 with sigma of 0.1
 C5, C11', S12', C13', C14', C15'
 with sigma of 0.1
 C101, C102, C103, C104, C105, C106, C107
 with sigma of 0.1
 C111, C112, C113, C114, C115, C116, C117
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C11')
Uanis(S12) = Uanis(C15')
Uanis(C13) = Uanis(C14')
Uanis(C14) = Uanis(C13')
Uanis(C15) = Uanis(S12')
5. Rigid body (RIGU) restrains
 C101, C102, C103, C104, C105, C106, C107, C111, C112, C113, C114, C115, C116,
 C117
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C11, S12, C13, C14, C15} sigma for 1-2: 0.005, 1-3: 0.005
as
{C11', S12', C13', C14', C15'}
7. Others
 Sof(C111)=Sof(C112)=Sof(H112)=Sof(C113)=Sof(H113)=Sof(C114)=Sof(H114)=
 Sof(C115)=Sof(H115)=Sof(C116)=Sof(H116)=Sof(C117)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=1-FVAR(1)
 Sof(C101)=Sof(C102)=Sof(H102)=Sof(C103)=Sof(H103)=Sof(C104)=Sof(H104)=
 Sof(C105)=Sof(H105)=Sof(C106)=Sof(H106)=Sof(C107)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=FVAR(1)
 Sof(C11')=Sof(S12')=Sof(C13')=Sof(H13')=Sof(C14')=Sof(H14')=Sof(C15')=
 Sof(H15')=1-FVAR(2)
 Sof(C11)=Sof(S12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C13'(H13'), C14'(H14'), C15'(H15'), C23(H23),
 C24(H24), C25(H25), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40),
  C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C102(H102),
 C103(H103), C104(H104), C105(H105), C106(H106), C112(H112), C113(H113),
 C114(H114), C115(H115), C116(H116)
8.b Fitted hexagon refined as free rotating group:
 C101(C102,C103,C104,C105,C106), C111(C112,C113,C114,C115,C116)
8.c Idealised Me refined as rotating group:
 C107(H10A,H10B,H10C), C117(H11A,H11B,H11C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'