Replacement of the phosphodiester backbone between canonical nucleosides with a dirhenium carbonyl "click" linker-a new class of luminescent organometallic dinucleoside phosphate mimics.
Skiba, Joanna; Kowalczyk, Aleksandra; Gorski, Aleksander; Dutkiewicz, Natalia; Gapińska, Magdalena; Stróżek, Józef; Woźniak, Krzysztof; Trzybiński, Damian; Kowalski, Konrad; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1551–1567; doi:10.1039/d2dt03995h

data_7712093
_publ_section_title
;
 Replacement of the phosphodiester backbone between canonical nucleosides
 with a dirhenium carbonyl "click" linker-a new class of luminescent
 organometallic dinucleoside phosphate mimics.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1551
_journal_page_last               1567
_journal_paper_doi               10.1039/d2dt03995h
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C17 H11 Cl2 N3 O6 Re2'
_chemical_formula_sum            'C17 H11 Cl2 N3 O6 Re2'
_chemical_formula_weight         796.59
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.439(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1476(4)
_cell_length_b                   6.13921(8)
_cell_length_c                   20.3399(4)
_cell_measurement_reflns_used    10827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.7960
_cell_measurement_theta_min      4.1820
_cell_volume                     2159.16(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -39.00   3.00   0.50    0.05    --    0.00 -44.00  94.00   84
  2  \w     52.00  85.00   0.50    0.05    --    0.00  44.00-114.00   66
  3  \w    -20.00  51.00   0.50    0.05    --    0.00  44.00-114.00  142
  4  \w    -80.00 -43.00   0.50    0.05    --    0.00-178.00 -60.00   74
  5  \w   -127.00 -12.00   0.50    0.20    --  -55.96 -44.00  94.00  230
  6  \w    -45.00  26.00   0.50    0.20    --  -55.96  44.00-114.00  142
  7  \w    -86.00 -24.00   0.50    0.20    --  -55.96 125.00-120.00  124
  8  \w   -133.00 -79.00   0.50    0.20    --  -55.96-125.00-150.00  108
  9  \w   -123.00 -96.00   0.50    0.20    --  -55.96 -99.00-150.00   54
 10  \w   -109.00 -25.00   0.50    0.20    --  -55.96 -57.00 -30.00  168
 11  \w   -121.00 -28.00   0.50    0.20    --  -55.96 -57.00   0.00  186
 12  \w    107.00 139.00   0.50    0.20    --   55.96 125.00-180.00   64
 13  \w     23.00 104.00   0.50    0.20    --   55.96  57.00 -90.00  162
 14  \w     51.00  76.00   0.50    0.20    --   55.96  44.00-114.00   50
 15  \w    122.00 178.00   0.50    1.00    --  111.93  44.00-114.00  112
 16  \w     28.00 155.00   0.50    1.00    --  111.93 -44.00  94.00  254
 17  \w    115.00 163.00   0.50    1.00    --  111.93  61.00 150.00   96
 18  \w     69.00  97.00   0.50    1.00    --  111.93  45.00 -30.00   56
 19  \w     56.00 146.00   0.50    1.00    --  111.93 -61.00-180.00  180
 20  \w    122.00 169.00   0.50    1.00    --  111.93  77.00  30.00   94
 21  \w     69.00  95.00   0.50    1.00    --  111.93  77.00 -60.00   52
 22  \w     52.00 105.00   0.50    1.00    --  111.93 -94.00  90.00  106
 23  \w     88.00 154.00   0.50    1.00    --  111.93  45.00 -60.00  132
 24  \w     62.00  87.00   0.50    1.00    --  111.93 -94.00 -60.00   50
 25  \w     69.00  95.00   0.50    1.00    --  111.93  77.00 -30.00   52
 26  \w     70.00  99.00   0.50    1.00    --  111.93  77.00  30.00   58
 27  \w     69.00 172.00   0.50    1.00    --  111.93  45.00  60.00  206
 28  \w    105.00 143.00   0.50    1.00    --  111.93 111.00-120.00   76
 29  \w     68.00 105.00   0.50    1.00    --  111.93  45.00   0.00   74
 30  \w     72.00  98.00   0.50    1.00    --  111.93  70.00 -10.93   52
 31  \w    101.00 151.00   0.50    1.00    --  111.93  70.00 -10.93  100
 32  \w     72.00 150.00   0.50    1.00    --  111.93  45.00  30.00  156
 33  \w    141.00 173.00   0.50    1.00    --  111.93  45.00 -30.00   64
 34  \w     67.00  92.00   0.50    1.00    --  111.93  42.00  62.65   50
 35  \w    111.00 166.00   0.50    1.00    --  111.93 111.00  60.00  110
 36  \w     63.00 146.00   0.50    1.00    --  111.93 178.00  90.00  166
 37  \w     78.00 105.00   0.50    1.00    --  111.93  61.00  30.00   54
 38  \w    103.00 153.00   0.50    1.00    --  111.93  77.00 -60.00  100
 39  \w     69.00  96.00   0.50    1.00    --  111.93  77.00   0.00   54
 40  \w     44.00  69.00   0.50    1.00    --  111.93  30.00  90.00   50
 41  \w     79.00 104.00   0.50    1.00    --  111.93  30.00  90.00   50
 42  \w    104.00 156.00   0.50    1.00    --  111.93 111.00 150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0388948000
_diffrn_orient_matrix_UB_12      0.1359644000
_diffrn_orient_matrix_UB_13      0.0386882000
_diffrn_orient_matrix_UB_21      0.0727687000
_diffrn_orient_matrix_UB_22      -0.0239901000
_diffrn_orient_matrix_UB_23      0.0725235000
_diffrn_orient_matrix_UB_31      0.0335526000
_diffrn_orient_matrix_UB_32      0.2095453000
_diffrn_orient_matrix_UB_33      -0.0167831000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17830
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         4.197
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.224
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.36a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.451
_exptl_crystal_description       needle
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+7.0123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3552
_reflns_number_total             3855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03995h2.cif
_cod_data_source_block           2022_02_16_dt_js-434b_n_auto
_cod_depositor_comments
'Adding full bibliography for 7712092--7712093.cif.'
_cod_original_cell_volume        2159.15(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7712093
_shelx_estimated_absorpt_t_max   0.572
_shelx_estimated_absorpt_t_min   0.068
_diffrn_oxdiff_digest_frames
;
0145de223eee0842602334deba5f37ab7304362da2d
;
_diffrn_oxdiff_digest_hkl
;
0187f0ae91bc673388d289021d55872a40fa4b
;
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4)
2.c :
 C8(H8), C11(H11)
;
_shelx_shelxl_version_number     2014/7
_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 1.459
_oxdiff_exptl_absorpt_empirical_full_min 0.772