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_7062664
_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, C4 H8 O'
_chemical_formula_sum            'C23 H24 N3 O7 Re'
_chemical_formula_weight         640.65
_chemical_name_common            jonrap11
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-09-27
_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                90
_cell_angle_beta                 96.0510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.08410(10)
_cell_length_b                   10.35030(10)
_cell_length_c                   15.17250(10)
_cell_measurement_reflns_used    26456
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.8450
_cell_measurement_theta_min      4.0760
_cell_volume                     2199.44(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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     25.00 120.00   0.50    0.05    --   47.28  77.00-150.00  190
  2  \w     32.00 120.00   0.50    0.05    --   47.28  57.00   0.00  176
  3  \w     34.00 120.00   0.50    0.05    --   47.28  47.00  79.00  172
  4  \w     29.00 120.00   0.50    0.05    --   47.28  66.00 109.24  182
  5  \w     25.00 120.00   0.50    0.05    --   47.28  77.00 150.00  190
  6  \w     91.00 178.00   0.50    0.05    --  113.25  77.00  30.00  174
  7  \w    100.00 178.00   0.50    0.05    --  113.25  47.00  79.00  156
  8  \w    101.00 178.00   0.50    0.05    --  113.25  45.00 120.00  154
  9  \w    101.00 178.00   0.50    0.05    --  113.25  45.00 150.00  154
 10  \w     97.00 178.00   0.50    0.05    --  113.25  61.00   0.00  162
 11  \w    100.00 178.00   0.50    0.05    --  113.25  15.00 -30.00  156
 12  \w    101.00 178.00   0.50    0.05    --  113.25  45.00-120.00  154
 13  \w    100.00 178.00   0.50    0.05    --  113.25  15.00-150.00  156
 14  \w     42.00  76.00   0.50    0.05    --  113.25 -61.00 -60.00   68
 15  \w     42.00  76.00   0.50    0.05    --  113.25 -61.00-180.00   68
 16  \w     42.00  76.00   0.50    0.05    --  113.25 -61.00-150.00   68
 17  \w     42.00  76.00   0.50    0.05    --  113.25 -61.00-120.00   68
 18  \w     42.00  76.00   0.50    0.05    --  113.25 -61.00  60.00   68
 19  \w     42.00  76.00   0.50    0.05    --  113.25 -61.00 120.00   68
 20  \w     42.00  76.00   0.50    0.05    --  113.25 -61.00 150.00   68
 21  \w     42.00  76.00   0.50    0.05    --  113.25 -61.00  90.00   68
 22  \w     42.00 106.00   0.50    0.05    --  113.25 -94.00  30.00  128
 23  \w     43.00 105.00   0.50    0.05    --  113.25 -96.00 171.02  124
 24  \w     43.00 106.00   0.50    0.05    --  113.25-101.00 -29.89  126
 25  \w     42.00 106.00   0.50    0.05    --  113.25 -94.00 -60.00  128
 26  \w     42.00 106.00   0.50    0.05    --  113.25 -94.00-150.00  128
 27  \w     34.00  93.00   0.50    0.05    --   47.28-125.00-150.00  118
 28  \w    -24.00  54.00   0.50    0.05    --   47.28 -47.00 -68.00  156
 29  \w    -27.00  18.00   0.50    0.05    --   47.28 -19.00 -60.00   90
 30  \w    -27.00  18.00   0.50    0.05    --   47.28 -19.00 120.00   90
 31  \w    -50.00  25.00   0.50    0.05    --  -47.28  47.00  79.00  150
 32  \w    -14.00  28.00   0.50    0.05    --  -47.28  19.00 -60.00   84
 33  \w    -14.00  28.00   0.50    0.05    --  -47.28  19.00-120.00   84
 34  \w    -14.00  28.00   0.50    0.05    --  -47.28  19.00-150.00   84
 35  \w    -47.00 -20.00   0.50    0.05    --  -91.75  45.00-150.00   54
 36  \w    -50.00 -19.00   0.50    0.05    --  -91.75  47.00  79.00   62
 37  \w   -119.00 -34.00   0.50    0.05    --  -47.28 -47.00 -68.00  170
 38  \w   -119.00 -32.00   0.50    0.05    --  -47.28 -57.00 -90.00  174
 39  \w   -119.00 -32.00   0.50    0.05    --  -47.28 -57.00-150.00  174
 40  \w   -163.00-114.00   0.50    0.05    --  -91.75 -76.00-110.93   98
 41  \w   -163.00 -79.00   0.50    0.05    --  -91.75 -47.00 -68.00  168
 42  \w   -163.00 -69.00   0.50    0.05    --  -91.75 -76.00  -6.36  188
;
_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      0.0595442000
_diffrn_orient_matrix_UB_12      -0.0860012000
_diffrn_orient_matrix_UB_13      0.0677754000
_diffrn_orient_matrix_UB_21      0.0791946000
_diffrn_orient_matrix_UB_22      -0.0082715000
_diffrn_orient_matrix_UB_23      -0.0624756000
_diffrn_orient_matrix_UB_31      0.0477767000
_diffrn_orient_matrix_UB_32      0.1212328000
_diffrn_orient_matrix_UB_33      0.0438660000
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38647
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.318
_diffrn_reflns_theta_min         4.074
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.263
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.64a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexane'
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0178P)^2^+8.5356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4660
_reflns_number_total             4762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02181e2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7062663--7062665.cif.'
_cod_database_code               7062664
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.292
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              12608
_olex2_submission_original_sample_id jonrap11
_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 1.645
_oxdiff_exptl_absorpt_empirical_full_min 0.765