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_1545604
_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, C21 H25 N6 Ni O2, 3(C2 H3 N)'
_chemical_formula_sum            'C27 H34 Br6 N9 Ni O2 Re'
_chemical_formula_weight         1241.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.166(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3999(4)
_cell_length_b                   23.9868(8)
_cell_length_c                   14.3655(6)
_cell_measurement_reflns_used    12973
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      30.6990
_cell_measurement_theta_min      5.3400
_cell_volume                     3927.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 0.814
_diffrn_measured_fraction_theta_max 0.758
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  27.00   1.00   10.00    --  -13.24 -99.00 -90.00   47
  2  \w    -20.00  55.00   1.00   10.00    --   14.65 -99.00   0.00   75
  3  \w     35.00 101.00   1.00   10.00    --   14.65 178.00 -30.00   66
  4  \w    -56.00  41.00   1.00   10.00    --   14.65 -57.00-150.00   97
  5  \w     -8.00  87.00   1.00   10.00    --   14.65  38.00 120.00   95
  6  \w    -59.00  46.00   1.00   10.00    --   14.65 -77.00 -60.00  105
  7  \w    -16.00  55.00   1.00   10.00    --   14.65 -99.00  60.00   71
  8  \w      5.00  47.00   1.00   10.00    --   14.65 -99.00-180.00   42
  9  \w     53.00  79.00   1.00   10.00    --   14.65  38.00   0.00   26
 10  \w    -52.00  37.00   1.00   10.00    --   14.65 -38.00 -60.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0041238000
_diffrn_orient_matrix_UB_12      0.0206349000
_diffrn_orient_matrix_UB_13      -0.0352364000
_diffrn_orient_matrix_UB_21      -0.0191974000
_diffrn_orient_matrix_UB_22      0.0196608000
_diffrn_orient_matrix_UB_23      0.0333049000
_diffrn_orient_matrix_UB_31      0.0590723000
_diffrn_orient_matrix_UB_32      0.0078172000
_diffrn_orient_matrix_UB_33      0.0094602000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.1061
_diffrn_reflns_Laue_measured_fraction_full 0.814
_diffrn_reflns_Laue_measured_fraction_max 0.758
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61149
_diffrn_reflns_point_group_measured_fraction_full 0.814
_diffrn_reflns_point_group_measured_fraction_max 0.758
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.165
_diffrn_reflns_theta_min         3.112
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.700
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    2.099
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.124
_refine_diff_density_max         2.693
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         9632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0333P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6105
_reflns_number_total             9632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00752c2.cif
_cod_data_source_block           eb17016_twin_comp1_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1545597--1545607.cif.'
_cod_database_code               1545604
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C27 H30 Br6 N9 Ni1 O2 Re1'
_chemical_oxdiff_usercomment     '@ 120 K AHP347'
_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), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              43487
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.074
_oxdiff_exptl_absorpt_empirical_full_min 0.549
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.9193\% 
 around [-0.00 0.00 1.00] (reciprocal) or [0.02 0.00 1.00] (direct)
;