Hexahalorhenate(iv) salts of metal oxazolidine nitroxides.
Pedersen, Anders H.; Geoghegan, Blaise L.; Nichol, Gary S.; Lupton, David W.; Murray, Keith S.; Martínez-Lillo, José; Gass, Ian A.; Brechin, Euan K.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5250–5259; doi:10.1039/c7dt00752c

data_1545602
_publ_section_title
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 Hexahalorhenate(iv) salts of metal oxazolidine nitroxides.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5250
_journal_page_last               5259
_journal_paper_doi               10.1039/c7dt00752c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'Cl6 Re, C30 H32 Co N6 O4, 4(C2 H3 N)'
_chemical_formula_sum            'C38 H44 Cl6 Co N10 O4 Re'
_chemical_formula_weight         1162.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.536(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5101(6)
_cell_length_b                   11.2475(4)
_cell_length_c                   15.7037(7)
_cell_measurement_reflns_used    8863
_cell_measurement_temperature    199.94(13)
_cell_measurement_theta_max      26.7660
_cell_measurement_theta_min      3.2260
_cell_volume                     2234.61(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.94(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.8207
_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    -20.00  30.00   1.00    5.00    --   -9.43 -99.00 -60.00   50
  2  \w    -20.00  30.00   1.00    5.00    --   -9.43 -99.00 120.00   50
  3  \w    -16.00  81.00   1.00    5.00    --   10.92  57.00 150.00   97
  4  \w    -62.00  33.00   1.00    5.00    --   10.92 -38.00-120.00   95
  5  \w    -59.00  38.00   1.00    5.00    --   10.92 -57.00   0.00   97
  6  \w    -20.00  51.00   1.00    5.00    --   10.92 -99.00 -90.00   71
  7  \w    -59.00  24.00   1.00    5.00    --   10.92 -57.00 -30.00   83
  8  \w    -12.00  78.00   1.00    5.00    --   10.92  38.00  60.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0476610000
_diffrn_orient_matrix_UB_12      -0.0038461000
_diffrn_orient_matrix_UB_13      -0.0119168000
_diffrn_orient_matrix_UB_21      -0.0055229000
_diffrn_orient_matrix_UB_22      0.0570093000
_diffrn_orient_matrix_UB_23      -0.0238869000
_diffrn_orient_matrix_UB_31      -0.0049821000
_diffrn_orient_matrix_UB_32      -0.0266807000
_diffrn_orient_matrix_UB_33      -0.0492693000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37200
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         3.220
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.488
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.204
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5470
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0712
_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^)+17.6831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4247
_reflns_number_total             5470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00752c2.cif
_cod_data_source_block           eb16206vt_200
_cod_depositor_comments
'Adding full bibliography for 1545597--1545607.cif.'
_cod_original_cell_volume        2234.61(17)
_cod_database_code               1545602
_chemical_oxdiff_formula         'C15 H16 Cl6 Co N3 O2 Re'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 N5, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C17, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C)
;
_shelx_res_checksum              57645
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.692
_oxdiff_exptl_absorpt_empirical_full_min 0.775