B-N-B Bond Embedded Phenalenyl and Its Anions.
Wei, Haipeng; Liu, Yulan; Gopalakrishna, Tullimilli Y.; Phan, Hoa; Huang, Xiaobo; Bao, Lipiao; Guo, Jing; Zhou, Jun; Luo, Shenglian; Wu, Jishan; Zeng, Zebing; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07375

data_4126649
_publ_section_title
;
 B-N-B Bond Embedded Phenalenyl and Its Anions.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07375
_journal_year                    2017
_chemical_formula_moiety         'C42 H63 B2 K2 N O12'
_chemical_formula_sum            'C42 H63 B2 K2 N O12'
_chemical_formula_weight         873.75
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.131(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.3567(6)
_cell_length_b                   12.1209(3)
_cell_length_c                   34.9719(11)
_cell_measurement_reflns_used    13328
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.4980
_cell_measurement_theta_min      4.3530
_cell_volume                     9039.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0697
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -32.00  54.00   1.00    1.00    --   34.73 -38.00  30.00   86
  2  \w     43.00  70.00   1.00    1.00    --   34.73 -99.00  30.00   27
  3  \w     -4.00  50.00   1.00    1.00    --   34.73 -57.00 150.00   54
  4  \w     44.00 125.00   1.00    4.00    --  107.46 -45.00  60.00   81
  5  \w     61.00  87.00   1.00    1.00    --   34.73  57.00 -30.00   26
  6  \w     23.00  67.00   1.00    1.00    --   34.73  57.00 -90.00   44
  7  \w     31.00 103.00   1.00    1.00    --   34.73  38.00-180.00   72
  8  \w     49.00  75.00   1.00    4.00    --  107.46 -61.00-120.00   26
  9  \w     55.00 122.00   1.00    4.00    --  107.46 -45.00-120.00   67
 10  \w     79.00 109.00   1.00    4.00    --  107.46 -94.00-150.00   30
 11  \w     43.00  86.00   1.00    4.00    --  107.46-111.00-120.00   43
 12  \w     41.00 123.00   1.00    4.00    --  107.46 -45.00 -30.00   82
 13  \w     58.00  84.00   1.00    1.00    --   34.73-125.00 -60.00   26
 14  \w     48.00  87.00   1.00    1.00    --   34.73-125.00-180.00   39
 15  \w     43.00 112.00   1.00    4.00    --  107.46 -45.00-180.00   69
 16  \w     38.00 176.00   1.00    4.00    --  107.46   0.00-180.00  138
 17  \w    107.00 138.00   1.00    4.00    --  107.46  88.00  27.00   31
 18  \w    101.00 132.00   1.00    4.00    --  107.46  61.00  30.00   31
 19  \w     64.00  97.00   1.00    4.00    --  107.46 178.00 -60.00   33
 20  \w     18.00 100.00   1.00    1.00    --   34.73  57.00  30.00   82
 21  \w     54.00  88.00   1.00    4.00    --  107.46 -77.00  30.00   34
 22  \w     37.00 110.00   1.00    4.00    --  107.46-111.00   0.00   73
 23  \w     39.00 115.00   1.00    4.00    --  107.46-111.00 120.00   76
 24  \w     60.00  96.00   1.00    4.00    --  107.46 -94.00 150.00   36
 25  \w    -27.00  53.00   1.00    1.00    --   34.73 -38.00-120.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0314250000
_diffrn_orient_matrix_UB_12      0.0529726000
_diffrn_orient_matrix_UB_13      0.0341229000
_diffrn_orient_matrix_UB_21      -0.0004223000
_diffrn_orient_matrix_UB_22      0.1125082000
_diffrn_orient_matrix_UB_23      -0.0205469000
_diffrn_orient_matrix_UB_31      -0.0649941000
_diffrn_orient_matrix_UB_32      -0.0262953000
_diffrn_orient_matrix_UB_33      -0.0190299000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            25956
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         4.20
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.985
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7988
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0853
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1313P)^2^+28.4644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2361
_reflns_number_gt                7069
_reflns_number_total             7988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b07375_si_005.cif
_cod_data_source_block           exp_170
_cod_database_code               4126649
_chemical_oxdiff_formula         'C40 H40 B2 N O6 K'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
O2 \\sim C19: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O5 \\sim C24: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C19) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C9(H9), C14(H14), C15(H15), C16(H16), C17(H17)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_olex2_date_sample_data_collection 2017-05-04
_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 2.406
_oxdiff_exptl_absorpt_empirical_full_min 0.401