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_1545599
_publ_section_title
;
 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         'Br6 Re, C30 H32 Co N6 O4'
_chemical_formula_sum            'C30 H32 Br6 Co N6 O4 Re'
_chemical_formula_weight         1265.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-04-08
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                106.156(3)
_cell_angle_beta                 101.328(3)
_cell_angle_gamma                93.673(3)
_cell_formula_units_Z            1
_cell_length_a                   8.1009(3)
_cell_length_b                   10.7229(3)
_cell_length_c                   10.9708(3)
_cell_measurement_reflns_used    10793
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.6660
_cell_measurement_theta_min      4.2820
_cell_volume                     890.35(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
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;
  1 omega -113.00  -17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega -113.00  -17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega  -75.00   31.00   1.0000    2.0000
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  6 omega   39.00  121.00   1.0000    8.0000
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  7 omega   40.00   99.00   1.0000    8.0000
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  8 omega   88.00  178.00   1.0000    8.0000
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  9 omega   87.00  178.00   1.0000    8.0000
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 10 omega   36.00   91.00   1.0000    8.0000
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    -      111.0000  -30.0000   30.0000 55

 11 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 79

 12 omega   39.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -90.0000 82

 13 omega   39.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 14 omega   87.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -180.0000 91

 15 omega   39.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 16 omega   39.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 82

 17 omega   40.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  120.0000 59

 18 omega   39.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 19 omega   66.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 20 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 21 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 79

 22 omega   36.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 55

 23 omega   40.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -120.0000 59

 24 omega   94.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -60.0000 84

 25 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 79

 26 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 79

 27 omega   94.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -90.0000 84

 28 omega -113.00  -17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000   30.0000 96

 29 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -120.0000 79

 30 omega -117.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  -30.0000 105

 31 omega -117.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000 -120.0000 105

 32 omega -117.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  120.0000 105

 33 omega -116.00  -21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -38.0000 -120.0000 95

 34 omega   87.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 35 omega   80.00  178.00   1.0000    8.0000
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 36 omega   83.00  178.00   1.0000    8.0000
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 37 omega   87.00  130.00   1.0000    8.0000
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 38 omega   83.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0753399000
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_diffrn_orient_matrix_UB_13      0.0493270000
_diffrn_orient_matrix_UB_21      -0.0859112000
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_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_theta_max         76.023
_diffrn_reflns_theta_min         4.305
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
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_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
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            'pale yellow'
_exptl_crystal_density_diffrn    2.360
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.0985
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_refine_diff_density_max         1.306
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_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0798P)^2^+0.1780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3462
_reflns_number_total             3700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00752c2.cif
_cod_data_source_block           eb16091_refinalized
_cod_depositor_comments
'Adding full bibliography for 1545597--1545607.cif.'
_cod_original_cell_volume        890.36(5)
_cod_database_code               1545599
_chemical_oxdiff_formula         'C15 H16 Br6 Co N3 O2'
_chemical_oxdiff_usercomment     '@ 120 K AHP348B'
_reflns_odcompleteness_completeness 100.00
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c)
;
_shelx_res_checksum              6907
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'