A polycyclic aromatic hydrocarbon diradical with pH-responsive magnetic properties.
Fu, Xiangyu; Han, Han; Zhang, Di; Yu, Han; He, Qilin; Zhao, Dahui; Chemical science 11 (2020) 5565–5571; doi:10.1039/d0sc00770f

data_1558047
_publ_section_title
;
 A polycyclic aromatic hydrocarbon diradical with pH-responsive magnetic
 properties.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              5565
_journal_page_last               5571
_journal_paper_doi               10.1039/d0sc00770f
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'B F4, C40 H35'
_chemical_formula_sum            'C40 H35 B F4'
_chemical_formula_weight         602.49
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-09 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.99110(10)
_cell_length_b                   34.2594(3)
_cell_length_c                   15.9758(2)
_cell_measurement_reflns_used    17522
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      74.6930
_cell_measurement_theta_min      3.1710
_cell_volume                     6255.29(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.960
_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     35.00 120.00   0.50    1.00    --   47.20  38.00 -60.00  170
  2  \w     83.00 169.00   0.50    3.00    --  103.25  90.00 -77.00  172
  3  \w    114.00 168.00   0.50    3.00    --  103.25 125.00 -30.00  108
  4  \w    105.00 166.00   0.50    3.00    --  103.25  45.00-120.00  122
  5  \w     92.00 157.00   0.50    3.00    --  103.25  30.00  30.00  130
  6  \w     87.00 130.00   0.50    3.00    --  103.25 -90.00 167.00   86
  7  \w     60.00  86.00   0.50    3.00    --  103.25 -90.00 167.00   52
  8  \w     32.00  97.00   0.50    3.00    --  103.25 -94.00 150.00  130
  9  \w     45.00 101.00   0.50    3.00    --  103.25 -94.00   0.00  112
 10  \w     13.00  73.00   0.50    1.00    --   47.20 -90.00 167.00  120
 11  \w    -49.00 -22.00   0.50    1.00    --  -47.20  90.00 -77.00   54
 12  \w    -70.00 -27.00   0.50    3.00    --  -99.00  90.00 -77.00   86
 13  \w   -117.00 -29.00   0.50    3.00    --  -99.00 125.00 -60.00  176
 14  \w   -162.00 -83.00   0.50    3.00    --  -99.00 -61.00-150.00  158
 15  \w   -120.00 -72.00   0.50    1.00    --  -47.20-125.00 -60.00   96
 16  \w   -103.00 -78.00   0.50    1.00    --  -47.20-125.00 -30.00   50
 17  \w   -120.00 -72.00   0.50    1.00    --  -47.20-125.00  60.00   96
 18  \w   -120.00 -85.00   0.50    3.00    --  -99.00 -61.00  30.00   70
 19  \w   -158.00-132.00   0.50    3.00    --  -99.00 -90.00 167.00   52
 20  \w   -167.00-141.00   0.50    3.00    --  -99.00 -61.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0036057000
_diffrn_orient_matrix_UB_12      -0.0291680000
_diffrn_orient_matrix_UB_13      -0.0741563000
_diffrn_orient_matrix_UB_21      0.0752483000
_diffrn_orient_matrix_UB_22      -0.0288234000
_diffrn_orient_matrix_UB_23      0.0679117000
_diffrn_orient_matrix_UB_31      -0.1117563000
_diffrn_orient_matrix_UB_32      -0.0184680000
_diffrn_orient_matrix_UB_33      0.0111932000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46687
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.565
_diffrn_reflns_theta_min         2.579
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       plate
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         12449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1674P)^2^+4.9372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2649
_refine_ls_wR_factor_ref         0.2848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9812
_reflns_number_total             12449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc00770f2.cif
_cod_data_source_block           tx1094
_cod_depositor_comments
;Adding full bibliography for 1558047.cif.

 Adding full bibliography for 1558047.cif.
;
_cod_database_code               1558047
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHF
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22), C22A(H22A)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C20(H20), C25(H25), C27(H27), C34(H34), C36(H36),
  C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C8A(H8A), C10A(H10A), C11A(H11A),
 C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C20A(H20A), C25A(H25A),
 C27A(H27A), C34A(H34A), C36A(H36A)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C29A(H29D,H29E,H29F),
 C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F), C38A(H38D,H38E,H38F), C39A(H39D,
 H39E,H39F), C40A(H40D,H40E,H40F)
;
_shelx_res_checksum              86000
_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 1.556
_oxdiff_exptl_absorpt_empirical_full_min 0.736