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_1545605
_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         'Cl6 Re, C30 H32 Co N6 O4, 2(C2 H3 N)'
_chemical_formula_sum            'C34 H38 Cl6 Co N8 O4 Re'
_chemical_formula_weight         1080.55
_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             2016-06-17
_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                80.2539(19)
_cell_angle_beta                 78.1007(19)
_cell_angle_gamma                88.8645(16)
_cell_formula_units_Z            1
_cell_length_a                   8.09457(16)
_cell_length_b                   10.9775(2)
_cell_length_c                   11.5719(3)
_cell_measurement_reflns_used    22407
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      37.4980
_cell_measurement_theta_min      3.5240
_cell_volume                     991.52(4)
_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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_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      120.01(10)
_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 0.961
_diffrn_measurement_details
;
  1 omega  -89.00  -29.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.1117  133.0000  -87.3350 120

  2 omega -115.00  -55.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.1117  178.0000  120.0000 120

  3 omega   -7.00   19.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.1117 -114.0000   56.4228 52

  4 omega  -20.00   71.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6742  -99.0000 -180.0000 182

  5 omega  -20.00   71.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6742  -99.0000   90.0000 182

  6 omega  -20.00   71.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6742  -99.0000   60.0000 182

  7 omega  -42.00   53.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6742  -38.0000 -120.0000 190

  8 omega  -56.00  117.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6742    0.0000  -90.0000 346

  9 omega    4.00  101.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6742   57.0000  -60.0000 194

 10 omega    4.00  101.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6742   57.0000 -180.0000 194

 11 omega    4.00   41.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6742   57.0000   30.0000 74
;
_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      -0.0484435000
_diffrn_orient_matrix_UB_12      -0.0524766000
_diffrn_orient_matrix_UB_13      0.0327737000
_diffrn_orient_matrix_UB_21      0.0698289000
_diffrn_orient_matrix_UB_22      -0.0384330000
_diffrn_orient_matrix_UB_23      -0.0152014000
_diffrn_orient_matrix_UB_31      0.0282576000
_diffrn_orient_matrix_UB_32      0.0082618000
_diffrn_orient_matrix_UB_33      0.0522862000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36771
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         37.651
_diffrn_reflns_theta_min         3.164
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.921
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.467
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       prism
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.3024
_exptl_crystal_size_mid          0.1101
_exptl_crystal_size_min          0.0836
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         10126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+0.2302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9918
_reflns_number_total             10126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00752c2.cif
_cod_data_source_block           eb16114_reint_refinalized
_cod_depositor_comments
'Adding full bibliography for 1545597--1545607.cif.'
_cod_original_cell_volume        991.53(4)
_cod_database_code               1545605
_chemical_oxdiff_formula         'C15 H16 Cl6 Co N3 O2 Re'
_chemical_oxdiff_usercomment     '@ 120 K AHP333 '
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Sof(N5)=1-FVAR(1)
 Sof(N4)=FVAR(1)
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)
;
_shelx_res_checksum              19286
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'