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_1545597
_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 Fe N6 O4'
_chemical_formula_sum            'C30 H32 Br6 Fe N6 O4 Re'
_chemical_formula_weight         1262.12
_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
;
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                105.576(5)
_cell_angle_beta                 101.890(5)
_cell_angle_gamma                93.681(4)
_cell_formula_units_Z            1
_cell_length_a                   8.0539(4)
_cell_length_b                   10.6650(6)
_cell_length_c                   11.0535(7)
_cell_measurement_reflns_used    3897
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.8700
_cell_measurement_theta_min      3.3750
_cell_volume                     887.72(9)
_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)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_details
;
  1 omega  -59.00   38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935  -57.0000   30.0000 97

  2 omega  -59.00   38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935  -57.0000 -120.0000 97

  3 omega  -20.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935   77.0000  -60.0000 105

  4 omega  -16.00   81.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935   57.0000 -180.0000 97

  5 omega  -16.00   81.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935   57.0000   30.0000 97

  6 omega  -20.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935  -99.0000  -30.0000 66

  7 omega  -20.00   51.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.9935  -99.0000 -180.0000 71
;
_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      0.0285498000
_diffrn_orient_matrix_UB_12      -0.0157371000
_diffrn_orient_matrix_UB_13      0.0586380000
_diffrn_orient_matrix_UB_21      0.0859301000
_diffrn_orient_matrix_UB_22      0.0189137000
_diffrn_orient_matrix_UB_23      -0.0003129000
_diffrn_orient_matrix_UB_31      -0.0057629000
_diffrn_orient_matrix_UB_32      0.0651111000
_diffrn_orient_matrix_UB_33      0.0353871000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15756
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.760
_diffrn_reflns_theta_min         3.077
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.612
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.299
_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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             597
_exptl_crystal_size_max          0.1998
_exptl_crystal_size_mid          0.0864
_exptl_crystal_size_min          0.0305
_refine_diff_density_max         2.010
_refine_diff_density_min         -1.893
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0272P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3685
_reflns_number_total             4460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00752c2.cif
_cod_data_source_block           eb16092_refinalized
_cod_depositor_comments
'Adding full bibliography for 1545597--1545607.cif.'
_cod_database_code               1545597
_chemical_oxdiff_formula         'C15 H16 Br6 Fe N3 O2 Re'
_chemical_oxdiff_usercomment     '@ 120 K AHP349B'
_reflns_odcompleteness_completeness 99.86
_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.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), 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              32170
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'