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_7062663
_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 H17 N3 O6 Re, Br'
_chemical_formula_sum            'C19 H17 Br N3 O6 Re'
_chemical_formula_weight         649.46
_chemical_name_common            jonrap04
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-28
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2023-05-11 deposited with the CCDC.	2023-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.2317(2)
_cell_length_b                   10.72530(10)
_cell_length_c                   20.2888(2)
_cell_measurement_reflns_used    37721
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      80.1530
_cell_measurement_theta_min      2.8770
_cell_volume                     4092.40(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (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 0.999
_diffrn_measured_fraction_theta_max 0.982
_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     27.00 120.00   0.50    0.12    --   47.27  72.00 176.00  186
  2  \w     35.00 120.00   0.50    0.12    --   47.27  38.00  90.00  170
  3  \w     32.00 118.00   0.50    0.12    --   47.27  57.00 -90.00  172
  4  \w     42.00 106.00   0.50    0.47    --  113.25 -94.00   0.00  128
  5  \w     42.00 111.00   0.50    0.47    --  113.25-125.00  60.00  138
  6  \w     42.00 111.00   0.50    0.47    --  113.25-125.00-150.00  138
  7  \w     42.00  80.00   0.50    0.47    --  113.25 -61.00-180.00   76
  8  \w     42.00  80.00   0.50    0.47    --  113.25 -61.00-120.00   76
  9  \w     42.00  80.00   0.50    0.47    --  113.25 -61.00 -90.00   76
 10  \w     42.00  80.00   0.50    0.47    --  113.25 -61.00 -60.00   76
 11  \w    -24.00  68.00   0.50    0.12    --   47.27 -72.00  46.00  184
 12  \w     42.00 134.00   0.50    0.47    --  113.25 -72.00  46.00  184
 13  \w     42.00  80.00   0.50    0.47    --  113.25 -61.00  60.00   76
 14  \w     42.00  80.00   0.50    0.47    --  113.25 -61.00  90.00   76
 15  \w     95.00 178.00   0.50    0.47    --  113.25 125.00 120.00  166
 16  \w    100.00 172.00   0.50    0.47    --  113.25  15.00  90.00  144
 17  \w     93.00 178.00   0.50    0.47    --  113.25  72.00 176.00  170
 18  \w     97.00 178.00   0.50    0.47    --  113.25  61.00 120.00  162
 19  \w    100.00 172.00   0.50    0.47    --  113.25  15.00 120.00  144
 20  \w     91.00 178.00   0.50    0.47    --  113.25  77.00 -90.00  174
 21  \w    100.00 172.00   0.50    0.47    --  113.25  15.00 -30.00  144
 22  \w    -68.00  25.00   0.50    0.12    --  -47.27  72.00 176.00  186
 23  \w   -112.00 -19.00   0.50    0.47    --  -91.75  72.00 176.00  186
 24  \w     -3.00  28.00   0.50    0.12    --  -47.27  19.00 -60.00   62
 25  \w    -73.00 -19.00   0.50    0.47    --  -91.75  61.00   0.00  108
 26  \w   -120.00 -27.00   0.50    0.12    --  -47.27 -72.00  46.00  186
 27  \w   -163.00 -71.00   0.50    0.47    --  -91.75 -72.00  46.00  184
 28  \w   -120.00 -73.00   0.50    0.12    --  -47.27-125.00-150.00   94
;
_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      -0.0742625000
_diffrn_orient_matrix_UB_12      -0.0428953000
_diffrn_orient_matrix_UB_13      -0.0373152000
_diffrn_orient_matrix_UB_21      -0.0024610000
_diffrn_orient_matrix_UB_22      0.1076681000
_diffrn_orient_matrix_UB_23      -0.0507475000
_diffrn_orient_matrix_UB_31      0.0344772000
_diffrn_orient_matrix_UB_32      -0.0848047000
_diffrn_orient_matrix_UB_33      -0.0454304000
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.217
_diffrn_reflns_theta_min         2.880
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.283
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
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    2.108
_exptl_crystal_description       block
_exptl_crystal_F_000             2480
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/diethyl ether'
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.251
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0299P)^2^+18.7825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8381
_reflns_number_total             8801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj02181e2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7062663--7062665.cif.'
_cod_database_code               7062663
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.277
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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), C23(H23), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C20(H20A,H20B), C22(H22A,H22B),
 C24(H24A,H24B)
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),
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35)
;
_shelx_res_checksum              9226
_olex2_submission_original_sample_id jonrap04
_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 1.223
_oxdiff_exptl_absorpt_empirical_full_min 0.869