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_1545601
_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, C21 H25 N6 Ni O2, C2 H3 N'
_chemical_formula_sum            'C23 H28 Cl6 N7 Ni O2 Re'
_chemical_formula_weight         892.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-08
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.0287(5)
_cell_length_b                   18.8615(4)
_cell_length_c                   22.0793(5)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.4040
_cell_measurement_theta_min      3.5100
_cell_volume                     6675.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -25.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1192  -99.0000   60.0000 45

  2 omega  -25.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1192  -99.0000  150.0000 45

  3 omega  -91.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1192    0.0000 -180.0000 142

  4 omega  -25.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1192  -99.0000  -90.0000 45

  5 omega   34.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8379  179.0000 -120.0000 62

  6 omega  -49.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8379  -38.0000    0.0000 93

  7 omega  -50.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8379  -19.0000  120.0000 110

  8 omega    3.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8379   57.0000   30.0000 87

  9 omega  -47.00    6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8379  -57.0000 -120.0000 53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0120267000
_diffrn_orient_matrix_UB_12      -0.0353279000
_diffrn_orient_matrix_UB_13      0.0066913000
_diffrn_orient_matrix_UB_21      0.0420903000
_diffrn_orient_matrix_UB_22      -0.0086116000
_diffrn_orient_matrix_UB_23      0.0066696000
_diffrn_orient_matrix_UB_31      -0.0065169000
_diffrn_orient_matrix_UB_32      0.0095718000
_diffrn_orient_matrix_UB_33      0.0307047000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78703
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.349
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.841
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.701
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.1123
_exptl_crystal_size_min          0.0904
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0157P)^2^+16.7649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5071
_reflns_number_total             6101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00752c2.cif
_cod_data_source_block           eb16060_refinalized
_cod_depositor_comments
'Adding full bibliography for 1545597--1545607.cif.'
_cod_database_code               1545601
_chemical_oxdiff_formula         'C15 H16 Cl6 N3 Ni O2 Re'
_chemical_oxdiff_usercomment     '@ 170 K AHP311B'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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)
;
_shelx_res_checksum              26547
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'