Chiral metal down to 4.2 K - a BDH-TTP radical-cation salt with spiroboronate anion B(2-chloromandelate)<sub>2</sub><sup/>.
Blundell, Toby J.; Brannan, Michael; Nishimoto, Hiroshi; Kadoya, Tomofumi; Yamada, Jun-Ichi; Akutsu, Hiroki; Nakazawa, Yasuhiro; Martin, Lee; Chemical communications (Cambridge, England) 57 (2021) 5406–5409; doi:10.1039/d1cc01441b

data_7128272
_publ_section_title
;
 Chiral metal down to 4.2 K - a BDH-TTP radical-cation salt with
 spiroboronate anion B(2-chloromandelate)<sub>2</sub><sup/>.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5406
_journal_page_last               5409
_journal_paper_doi               10.1039/d1cc01441b
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C16 H10 B Cl2 O6, 2(C10 H8 S8)'
_chemical_formula_sum            'C36 H26 B Cl2 O6 S16'
_chemical_formula_weight         1149.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-11 deposited with the CCDC.	2021-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.546(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0733(7)
_cell_length_b                   8.0039(4)
_cell_length_c                   24.5775(11)
_cell_measurement_reflns_used    5625
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.4170
_cell_measurement_theta_min      3.7180
_cell_volume                     2148.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.894
_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      3.00  83.00   1.00   17.38    --   20.20  57.00 -30.00   80
  2  \w      6.00  86.00   1.00   17.38    --   20.20  57.00-120.00   80
  3  \w    -46.00 -20.00   1.00   17.38    --   20.20 -57.00 -30.00   26
  4  \w      4.00  71.00   1.00   17.38    --   20.20  57.00  60.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0203063000
_diffrn_orient_matrix_UB_12      0.0155444000
_diffrn_orient_matrix_UB_13      0.0254116000
_diffrn_orient_matrix_UB_21      0.0613577000
_diffrn_orient_matrix_UB_22      0.0134070000
_diffrn_orient_matrix_UB_23      0.0128514000
_diffrn_orient_matrix_UB_31      -0.0059113000
_diffrn_orient_matrix_UB_32      0.0863273000
_diffrn_orient_matrix_UB_33      -0.0066231000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            13309
_diffrn_reflns_point_group_measured_fraction_full 0.789
_diffrn_reflns_point_group_measured_fraction_max 0.652
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.768
_diffrn_reflns_theta_min         3.345
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       plate
_exptl_crystal_F_000             1170
_exptl_crystal_recrystallization_method electrocrystallisation
_exptl_crystal_size_max          0.382
_exptl_crystal_size_mid          0.341
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 1932 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_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     570
_refine_ls_number_reflns         8751
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0373P)^2^+0.4673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.371
_reflns_Friedel_fraction_full    0.546
_reflns_Friedel_fraction_max     0.377
_reflns_number_gt                7783
_reflns_number_total             8751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01441b2.cif
_cod_data_source_block           mb6full
_cod_depositor_comments          'Adding full bibliography for 7128272.cif.'
_cod_database_code               7128272
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C36H26BCl2O6S16
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.706
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(1)
 Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(2)
 Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C22(H22), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C9A(H9AA,H9AB),
 C10A(H10C,H10D), C11(H11A,H11B), C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B)
3.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C28(H28), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              23304
_shelx_hkl_checksum              4028
_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 1.099
_oxdiff_exptl_absorpt_empirical_full_min 0.902