An unprecedented pyridine-based dinuclear mixed-valent Re<sup>I/VII</sup> oxo-bridged complex: a solvatochromic and AIE-active probe for nanomolar detection of picric acid and trinitrotoluene.
Mukherjee, Atasi; Bhattacharya, Suman; Chakravarty, Manab; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9144–9157; doi:10.1039/d1dt01002f

data_7707457
_publ_section_title
;
 An unprecedented pyridine-based dinuclear mixed-valent Re<sup>I/VII</sup>
 oxo-bridged complex: a solvatochromic and AIE-active probe for nanomolar
 detection of picric acid and trinitrotoluene.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9144
_journal_page_last               9157
_journal_paper_doi               10.1039/d1dt01002f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C59 H42 N2 O9 Re2'
_chemical_formula_sum            'C59 H42 N2 O9 Re2'
_chemical_formula_weight         1295.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                73.5073(13)
_cell_angle_beta                 86.5828(12)
_cell_angle_gamma                88.1763(12)
_cell_formula_units_Z            2
_cell_length_a                   8.44843(12)
_cell_length_b                   17.0812(3)
_cell_length_c                   18.8380(3)
_cell_measurement_reflns_used    18750
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      79.3350
_cell_measurement_theta_min      4.1180
_cell_volume                     2601.70(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -89.00   1.00   0.50    0.60    --    0.00 -37.00  30.00  180
  2  \w    -24.00  17.00   0.50    0.60    --    0.00 -37.00 120.00   82
  3  \w    -88.00 -35.00   0.50    0.60    --    0.00 -37.00 120.00  106
  4  \w    -19.00  30.00   0.50    0.60    --    0.00 -77.00  90.00   98
  5  \w    -89.00 -57.00   0.50    0.60    --    0.00 -77.00   0.00   64
  6  \w    -37.00  28.00   0.50    0.60    --    0.00 -77.00   0.00  130
  7  \w    -89.00 -59.00   0.50    0.60    --    0.00 -77.00  90.00   60
  8  \w     81.00 196.00   0.50    2.42    --  107.20  15.00 -90.00  230
  9  \w     61.00  98.00   0.50    2.42    --  107.20 -82.00 150.00   74
 10  \w     21.00 131.00   0.50    2.42    --  107.20 -61.00  30.00  220
 11  \w     32.00 140.00   0.50    2.42    --  107.20 -82.00-120.00  216
 12  \w     88.00 114.00   0.50    2.42    --  107.20  30.00 -30.00   52
 13  \w    136.00 189.00   0.50    2.42    --  107.20  30.00 -30.00  106
 14  \w     87.00 112.00   0.50    2.42    --  107.20 -82.00 -60.00   50
 15  \w     99.00 125.00   0.50    2.42    --  107.20 -61.00-120.00   52
 16  \w     80.00 140.00   0.50    2.42    --  107.20 -82.00 120.00  120
 17  \w     18.00 135.00   0.50    2.42    --  107.20 -15.00-120.00  234
 18  \w     21.00  58.00   0.50    2.42    --  107.20 -45.00 -60.00   74
 19  \w     31.00 121.00   0.50    2.42    --  107.20 -82.00  30.00  180
 20  \w     38.00  98.00   0.50    2.42    --  107.20 -61.00-120.00  120
 21  \w     94.00 125.00   0.50    2.42    --  107.20 -45.00  30.00   62
 22  \w     20.00 109.00   0.50    2.42    --  107.20 -82.00-180.00  178
 23  \w     38.00  93.00   0.50    2.42    --  107.20 -45.00  30.00  110
 24  \w     89.00 114.00   0.50    2.42    --  107.20  30.00  60.00   50
 25  \w    131.00 157.00   0.50    2.42    --  107.20  30.00  60.00   52
 26  \w     24.00 125.00   0.50    2.42    --  107.20 -30.00 150.00  202
 27  \w     82.00 107.00   0.50    2.42    --  107.20 -82.00  -4.46   50
 28  \w     84.00 109.00   0.50    2.42    --  107.20 -82.00 -30.00   50
 29  \w    104.00 130.00   0.50    2.42    --  107.20 -82.00  90.00   52
 30  \w     42.00  67.00   0.50    2.42    --  107.20 -82.00  -4.46   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0970954000
_diffrn_orient_matrix_UB_12      -0.0733869000
_diffrn_orient_matrix_UB_13      0.0468044000
_diffrn_orient_matrix_UB_21      -0.1345014000
_diffrn_orient_matrix_UB_22      0.0245150000
_diffrn_orient_matrix_UB_23      -0.0541725000
_diffrn_orient_matrix_UB_31      0.0765483000
_diffrn_orient_matrix_UB_32      -0.0535065000
_diffrn_orient_matrix_UB_33      -0.0465738000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31039
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.206
_diffrn_reflns_theta_min         4.127
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.441
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         10.155
_refine_diff_density_min         -4.726
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         10952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0791
_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^)+(0.1093P)^2^+33.5189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9726
_reflns_number_total             10952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01002f2.cif
_cod_data_source_block           exp_567_re-an-4py-dec_sq
_cod_depositor_comments
'Adding full bibliography for 7707456--7707457.cif.'
_cod_database_code               7707457
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.185
_shelx_estimated_absorpt_t_min   0.124
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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. Uiso/Uaniso restraints and constraints
Uiso(C56B) = Uiso(C56A)
3. Others
 Sof(C54B)=Sof(H54B)=Sof(C55B)=Sof(H55B)=Sof(C51B)=Sof(H51B)=Sof(C53B)=
 Sof(C52B)=Sof(H52B)=Sof(O2B)=Sof(C56B)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1)
 Sof(C56A)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(O2A)=Sof(C55A)=Sof(H55A)=
 Sof(C51A)=Sof(H51A)=Sof(C52A)=Sof(H52A)=Sof(C54A)=Sof(H54A)=Sof(C53A)=FVAR(1)
 Sof(C5B)=Sof(H5B)=Sof(C4B)=Sof(H4B)=Sof(C7B)=Sof(H7B)=Sof(C6B)=Sof(H6B)=
 Sof(C3B)=Sof(N1B)=Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2B)=1-FVAR(2)
 Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C3A)=Sof(C2A)=Sof(H2A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C13(H13), C30(H30), C33(H33), C34(H34), C26(H26), C41(H41),
 C12(H12), C29(H29), C27(H27), C35(H35), C40(H40), C17(H17), C39(H39), C23(H23),
  C38(H38), C11(H11), C5B(H5B), C48(H48), C1A(H1A), C18(H18), C10(H10),
 C20(H20), C47(H47), C4B(H4B), C19(H19), C24(H24), C54B(H54B), C45(H45),
 C55B(H55B), C46(H46), C7B(H7B), C51B(H51B), C52B(H52B), C2A(H2A), C6B(H6B),
 C55A(H55A), C51A(H51A), C52A(H52A), C54A(H54A), C4A(H4A), C5A(H5A), C1B(H1B),
 C2B(H2B), C6A(H6A), C7A(H7A)
4.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C56A(H56A,H56B,H56C), C56B(H56D,H56E,H56F)
;
_shelx_res_checksum              1530
_shelx_hkl_checksum              33064
_shelx_fab_checksum              60940
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.982
_oxdiff_exptl_absorpt_empirical_full_min 0.496