Synthesis, characterization, and structure determination of bis-oxazolidine complexes of rhenium
Pohorenec, Ryan A.; Brennessel, William W.; Jones, William D.; New Journal of Chemistry 47 (2023) 16872–16878; doi:10.1039/D3NJ02181E

data_7062665
_publ_section_title
;
 Synthesis, characterization, and structure determination of
 bis-oxazolidine complexes of rhenium
;
_journal_issue                   36
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16872
_journal_page_last               16878
_journal_paper_doi               10.1039/D3NJ02181E
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C19 H16 N3 O6 Re'
_chemical_formula_sum            'C19 H16 N3 O6 Re'
_chemical_formula_weight         568.55
_chemical_name_common            jonrap12
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-12-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-11 deposited with the CCDC.	2023-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                81.8090(10)
_cell_angle_beta                 81.8630(10)
_cell_angle_gamma                81.9800(10)
_cell_formula_units_Z            4
_cell_length_a                   10.03030(10)
_cell_length_b                   10.4951(2)
_cell_length_c                   17.6513(2)
_cell_measurement_reflns_used    37583
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.9030
_cell_measurement_theta_min      4.2760
_cell_volume                     1807.11(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_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    -14.00  28.00   0.50    0.06    --  -47.28  19.00  60.00   84
  2  \w    -14.00  28.00   0.50    0.06    --  -47.28  19.00  30.00   84
  3  \w    -14.00  28.00   0.50    0.06    --  -47.28  19.00   0.00   84
  4  \w    -14.00  28.00   0.50    0.06    --  -47.28  19.00 -60.00   84
  5  \w    -14.00  28.00   0.50    0.06    --  -47.28  19.00-120.00   84
  6  \w    -14.00  28.00   0.50    0.06    --  -47.28  19.00-150.00   84
  7  \w    -14.00  28.00   0.50    0.06    --  -47.28  19.00 150.00   84
  8  \w     25.00 120.00   0.50    0.06    --   47.28  77.00 -30.00  190
  9  \w     25.00 120.00   0.50    0.06    --   47.28  77.00 -60.00  190
 10  \w     25.00 120.00   0.50    0.06    --   47.28  77.00-180.00  190
 11  \w     25.00 120.00   0.50    0.06    --   47.28  77.00-120.00  190
 12  \w     25.00 120.00   0.50    0.06    --   47.28  77.00  30.00  190
 13  \w     25.00 120.00   0.50    0.06    --   47.28  77.00 150.00  190
 14  \w     25.00 120.00   0.50    0.06    --   47.28  77.00  90.00  190
 15  \w     35.00 120.00   0.50    0.06    --   47.28  38.00 120.00  170
 16  \w     32.00 120.00   0.50    0.06    --   47.28  57.00  30.00  176
 17  \w     35.00 120.00   0.50    0.06    --   47.28  38.00 -30.00  170
 18  \w     35.00 120.00   0.50    0.06    --   47.28  38.00 -90.00  170
 19  \w     35.00 120.00   0.50    0.06    --   47.28  38.00-180.00  170
 20  \w    100.00 178.00   0.50    0.22    --  113.25  15.00 -60.00  156
 21  \w    101.00 178.00   0.50    0.22    --  113.25  45.00-150.00  154
 22  \w     97.00 178.00   0.50    0.22    --  113.25  61.00 -30.00  162
 23  \w     97.00 178.00   0.50    0.22    --  113.25  61.00  30.00  162
 24  \w    101.00 178.00   0.50    0.22    --  113.25  45.00  90.00  154
 25  \w    100.00 178.00   0.50    0.22    --  113.25  15.00 150.00  156
 26  \w    101.00 178.00   0.50    0.22    --  113.25  45.00  60.00  154
 27  \w    101.00 178.00   0.50    0.22    --  113.25  45.00   0.00  154
 28  \w    100.00 178.00   0.50    0.22    --  113.25  15.00-120.00  156
 29  \w    100.00 178.00   0.50    0.22    --  113.25  15.00-180.00  156
 30  \w     95.00 178.00   0.50    0.22    --  113.25 125.00 -90.00  166
 31  \w    101.00 178.00   0.50    0.22    --  113.25  89.00-116.00  154
 32  \w     42.00  76.00   0.50    0.22    --  113.25 -61.00-180.00   68
 33  \w     42.00  76.00   0.50    0.22    --  113.25 -61.00-150.00   68
 34  \w     42.00  76.00   0.50    0.22    --  113.25 -61.00 -90.00   68
 35  \w     42.00  76.00   0.50    0.22    --  113.25 -61.00 -30.00   68
 36  \w     42.00  76.00   0.50    0.22    --  113.25 -61.00  60.00   68
 37  \w     42.00  76.00   0.50    0.22    --  113.25 -61.00 120.00   68
 38  \w     34.00  93.00   0.50    0.06    --   47.28-125.00 150.00  118
 39  \w     44.00 111.00   0.50    0.22    --  113.25-125.00  60.00  134
 40  \w     44.00 111.00   0.50    0.22    --  113.25-125.00   0.00  134
 41  \w     42.00 106.00   0.50    0.22    --  113.25 -94.00  90.00  128
 42  \w     44.00 111.00   0.50    0.22    --  113.25-125.00 -60.00  134
 43  \w     45.00 110.00   0.50    0.22    --  113.25-119.00-137.63  130
 44  \w     42.00 106.00   0.50    0.22    --  113.25 -94.00-180.00  128
 45  \w     42.00 106.00   0.50    0.22    --  113.25 -94.00-120.00  128
 46  \w     42.00 106.00   0.50    0.22    --  113.25 -94.00 -60.00  128
 47  \w     42.00 106.00   0.50    0.22    --  113.25 -94.00-150.00  128
 48  \w     42.00 106.00   0.50    0.22    --  113.25 -94.00   0.00  128
 49  \w     42.00 106.00   0.50    0.22    --  113.25 -94.00  30.00  128
 50  \w     42.00 106.00   0.50    0.22    --  113.25 -94.00  60.00  128
 51  \w     42.00 106.00   0.50    0.22    --  113.25 -94.00 120.00  128
 52  \w     42.00 106.00   0.50    0.22    --  113.25 -89.00 128.00  128
 53  \w    -20.00  76.00   0.50    0.06    --   47.28 -89.00 128.00  192
 54  \w    -47.00 -20.00   0.50    0.22    --  -91.75  45.00  30.00   54
 55  \w    -75.00  25.00   0.50    0.06    --  -47.28  89.00-116.00  200
 56  \w    -80.00 -19.00   0.50    0.22    --  -91.75  89.00-116.00  122
 57  \w    -47.00 -20.00   0.50    0.22    --  -91.75  45.00  90.00   54
 58  \w   -163.00 -79.00   0.50    0.22    --  -91.75 -89.00 128.00  168
 59  \w   -163.00 -70.00   0.50    0.22    --  -91.75 -75.00 142.56  186
 60  \w   -163.00 -69.00   0.50    0.22    --  -91.75 -77.00 105.23  188
 61  \w   -163.00 -69.00   0.50    0.22    --  -91.75 -77.00  30.00  188
 62  \w   -163.00 -70.00   0.50    0.22    --  -91.75 -74.00 -40.75  186
 63  \w   -163.00 -71.00   0.50    0.22    --  -91.75 -71.00 -11.33  184
 64  \w   -163.00 -71.00   0.50    0.22    --  -91.75 -71.00  62.98  184
 65  \w   -163.00 -71.00   0.50    0.22    --  -91.75 -71.00 -63.27  184
 66  \w   -163.00 -74.00   0.50    0.22    --  -91.75 -63.00-104.17  178
 67  \w   -163.00 -69.00   0.50    0.22    --  -91.75 -76.00-167.99  188
 68  \w   -163.00 -70.00   0.50    0.22    --  -91.75 -75.00-132.21  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0075460000
_diffrn_orient_matrix_UB_12      0.0383126000
_diffrn_orient_matrix_UB_13      0.0802170000
_diffrn_orient_matrix_UB_21      -0.1537324000
_diffrn_orient_matrix_UB_22      0.0447522000
_diffrn_orient_matrix_UB_23      0.0085393000
_diffrn_orient_matrix_UB_31      -0.0272797000
_diffrn_orient_matrix_UB_32      -0.1373103000
_diffrn_orient_matrix_UB_33      0.0372719000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61205
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.228
_diffrn_reflns_theta_min         4.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.913
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7771
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0297P)^2^+5.6070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7396
_reflns_number_total             7771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02181e2.cif
_cod_data_source_block           10b
_cod_depositor_comments
'Adding full bibliography for 7062663--7062665.cif.'
_cod_database_code               7062665
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.330
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Re2-O7 \\sim Re2-O7A
 with sigma of 0.02
 O7-C20 \\sim O7A-C20A
 with sigma of 0.02
 O9-C21 \\sim O9A-C21
 with sigma of 0.04
 O8-C22 \\sim O8A-C22A
 with sigma of 0.02
 O7-C21 \\sim O7A-C21
 with sigma of 0.04
 O9-C24 \\sim O9A-C24A
 with sigma of 0.02
 O8-C23 \\sim O8A-C23
 with sigma of 0.02
 O9-C25 \\sim O9A-C25
 with sigma of 0.02
 Re2-C20 \\sim Re2-C20A
 with sigma of 0.04
 C20-C21 \\sim C20A-C21
 with sigma of 0.02
 O8-C21 \\sim O8A-C21
 with sigma of 0.04
 C21-C22 \\sim C21-C22A
 with sigma of 0.02
 C22-C23 \\sim C22A-C23
 with sigma of 0.04
 C21-C24 \\sim C21-C24A
 with sigma of 0.02
 C24-C25 \\sim C24A-C25
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.003 and sigma
for terminal atoms of 0.006 within 1A
Uanis(C20A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(H23A)=Sof(H25A)=Sof(O9A)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C22A)=
 Sof(H22C)=Sof(H22D)=Sof(O8A)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(O7A)=1-FVAR(1)
 Sof(O7)=Sof(O8)=Sof(O9)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H25)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C23(H23), C23(H23A), C25(H25), C25(H25A), C6(H6), C4(H4)
5.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B), C5(H5A,H5B), C1(H1A,H1B),
 C3(H3A,H3B), C24A(H24C,H24D), C22A(H22C,H22D), C20A(H20C,H20D)
5.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C9(H9), C14(H14), C11(H11), C8(H8), C10(H10), C13(H13), C15(H15),
 C16(H16)
;
_shelx_res_checksum              27979
_olex2_submission_original_sample_id jonrap12
_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 1.192
_oxdiff_exptl_absorpt_empirical_full_min 0.792