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_1545607
_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 Cu N6 O4'
_chemical_formula_sum            'C30 H32 Cl6 Cu N6 O4 Re'
_chemical_formula_weight         1003.05
_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                107.565(3)
_cell_angle_beta                 102.333(2)
_cell_angle_gamma                93.278(2)
_cell_formula_units_Z            1
_cell_length_a                   8.0389(2)
_cell_length_b                   10.6038(3)
_cell_length_c                   10.8240(3)
_cell_measurement_reflns_used    11493
_cell_measurement_temperature    119.93(17)
_cell_measurement_theta_max      76.0250
_cell_measurement_theta_min      4.3900
_cell_volume                     851.99(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)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.93(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
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_diffrn_measurement_details
;
  1 omega -113.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000   90.0000 96

  2 omega  -96.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega -113.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000 -150.0000 96

  4 omega  -70.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   57.0000    0.0000 97

  5 omega   23.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000 -180.0000 75

  6 omega   40.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -60.0000 58

  7 omega   40.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   60.0000 58

  8 omega   87.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -30.0000 91

  9 omega   87.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   30.0000 91

 10 omega   87.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -90.0000 91

 11 omega   30.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 79

 12 omega   36.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 55

 13 omega   30.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 79

 14 omega   87.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -120.0000 91

 15 omega   39.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 82

 16 omega   40.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  120.0000 58

 17 omega   39.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 82

 18 omega   30.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 79

 19 omega   94.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -90.0000 84

 20 omega   30.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 79

 21 omega   30.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 79

 22 omega   40.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -180.0000 58

 23 omega   39.00  120.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -121.0000  -74.3829 81

 24 omega -117.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  150.0000 105

 25 omega -117.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  -60.0000 105

 26 omega -117.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000   60.0000 105

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

 28 omega   23.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000  -90.0000 75

 29 omega   83.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 95

 30 omega   66.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  150.0000 112

 31 omega   87.00  143.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -180.0000 56
;
_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      0.0389364000
_diffrn_orient_matrix_UB_12      0.1033416000
_diffrn_orient_matrix_UB_13      -0.0674611000
_diffrn_orient_matrix_UB_21      0.1600964000
_diffrn_orient_matrix_UB_22      0.0640332000
_diffrn_orient_matrix_UB_23      0.1150558000
_diffrn_orient_matrix_UB_31      0.1095514000
_diffrn_orient_matrix_UB_32      -0.0940520000
_diffrn_orient_matrix_UB_33      -0.0767558000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13972
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.269
_diffrn_reflns_theta_min         4.411
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34335
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_description       plate
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.1824
_exptl_crystal_size_mid          0.1109
_exptl_crystal_size_min          0.0264
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0195
_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^)+(0.0295P)^2^+0.4866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3495
_reflns_number_total             3525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00752c2.cif
_cod_data_source_block           eb4301_refinalized
_cod_depositor_comments
'Adding full bibliography for 1545597--1545607.cif.'
_cod_original_cell_volume        851.99(5)
_cod_database_code               1545607
_chemical_oxdiff_formula         'C16 H16 Cl6 Cu N3 O2 Re'
_chemical_oxdiff_usercomment     '@ 120 K AHP196'
_reflns_odcompleteness_completeness 99.97
_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. Others
 Sof(C12)=Sof(H12A)=Sof(H12B)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(1)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=1-FVAR(2)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C16(H16A,H16B)
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              15125
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'