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_1545603
_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 Fe N6 O4'
_chemical_formula_sum            'C30 H32 Cl6 Fe N6 O4 Re'
_chemical_formula_weight         995.36
_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                106.255(4)
_cell_angle_beta                 103.909(3)
_cell_angle_gamma                92.852(3)
_cell_formula_units_Z            1
_cell_length_a                   7.9831(3)
_cell_length_b                   10.5052(5)
_cell_length_c                   10.7890(4)
_cell_measurement_reflns_used    6194
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      27.9490
_cell_measurement_theta_min      3.3430
_cell_volume                     836.49(6)
_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)
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_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 0.993
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_details
;
  1 omega  -20.00   33.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -99.0000  120.0000 53

  2 omega  -20.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -99.0000  -60.0000 69

  3 omega  -20.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -99.0000 -150.0000 69

  4 omega  -14.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196   38.0000  150.0000 95

  5 omega  -78.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196    0.0000  150.0000 173

  6 omega  -65.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -77.0000   60.0000 105
;
_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      -0.0310039000
_diffrn_orient_matrix_UB_12      -0.0613222000
_diffrn_orient_matrix_UB_13      0.0071157000
_diffrn_orient_matrix_UB_21      0.0867834000
_diffrn_orient_matrix_UB_22      -0.0141311000
_diffrn_orient_matrix_UB_23      0.0190459000
_diffrn_orient_matrix_UB_31      0.0044929000
_diffrn_orient_matrix_UB_32      0.0326425000
_diffrn_orient_matrix_UB_33      0.0680517000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13462
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.783
_diffrn_reflns_theta_min         3.132
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.575
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.618
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       plate
_exptl_crystal_F_000             489
_exptl_crystal_size_max          0.1579
_exptl_crystal_size_mid          0.0949
_exptl_crystal_size_min          0.0337
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0173P)^2^+0.4376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3586
_reflns_number_total             3822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00752c2.cif
_cod_data_source_block           eb16062_refinalized
_cod_depositor_comments
'Adding full bibliography for 1545597--1545607.cif.'
_cod_database_code               1545603
_chemical_oxdiff_formula         'C15 H16 Cl6 Fe N3 O2 Re'
_chemical_oxdiff_usercomment     '@ 120 K AHP335C'
_reflns_odcompleteness_completeness 98.80
_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(C16)=Sof(H16a)=Sof(H16b)=1-FVAR(1)
 Sof(C12)=Sof(H12a)=Sof(H12b)=FVAR(1)
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)
;
_shelx_res_checksum              83349
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'