Incorporation of H<sub>2</sub>O and CO<sub>2</sub> into a BN-embedded 3<i>aH</i>-3<i>a</i><sup>1</sup><i>H</i>-acephenanthrylene derivative.
Guo, Rui; Jiang, Jingxing; Ke, Zhuofeng; Tung, Chen-Ho; Kong, Lingbing; Chemical communications (Cambridge, England) 57 (2021) 1226–1229; doi:10.1039/d0cc07276a

data_7127711
_publ_section_title
;
 Incorporation of H<sub>2</sub>O and CO<sub>2</sub> into a BN-embedded
 3<i>aH</i>-3<i>a</i><sup>1</sup><i>H</i>-acephenanthrylene derivative.
;
_journal_issue                   10
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1226
_journal_page_last               1229
_journal_paper_doi               10.1039/d0cc07276a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C48 H52 B2 N2 O, C7 H8'
_chemical_formula_sum            'C55 H60 B2 N2 O'
_chemical_formula_weight         786.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-02 deposited with the CCDC.	2020-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                111.154(3)
_cell_angle_beta                 91.945(3)
_cell_angle_gamma                97.305(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6024(4)
_cell_length_b                   12.4641(4)
_cell_length_c                   17.0448(5)
_cell_measurement_reflns_used    7301
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      72.1650
_cell_measurement_theta_min      3.7880
_cell_volume                     2271.64(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.19a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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     54.00  80.00   1.00    5.50    --   98.46 -29.00 -17.00   26
  2  \w     28.00 112.00   1.00    5.50    --   98.46 -57.00   0.00   84
  3  \w     58.00 118.00   1.00    0.80    --   48.45  29.00 144.00   60
  4  \w     87.00 173.00   1.00    5.50    --   98.46  29.00 144.00   86
  5  \w     26.00 106.00   1.00    5.50    --   98.46 -99.00  30.00   80
  6  \w     23.00 111.00   1.00    5.50    --   98.46 -19.00 150.00   88
  7  \w    -24.00   4.00   1.00    0.80    --   48.45 -29.00 -17.00   28
  8  \w     37.00 114.00   1.00    5.50    --   98.46-125.00-150.00   77
  9  \w     26.00 109.00   1.00    5.50    --   98.46 -99.00-150.00   83
 10  \w    -60.00  22.00   1.00    0.80    --  -48.45  29.00 144.00   82
 11  \w    -94.00 -14.00   1.00    5.50    --  -86.25  29.00 144.00   80
 12  \w   -100.00 -21.00   1.00    5.50    --  -86.25  77.00 -30.00   79
 13  \w   -101.00 -15.00   1.00    5.50    --  -86.25  57.00 -30.00   86
 14  \w    -98.00 -13.00   1.00    5.50    --  -86.25  37.00 -60.00   85
 15  \w   -121.00 -42.00   1.00    0.80    --  -48.45 -29.00 -17.00   79
 16  \w   -103.00 -72.00   1.00    0.80    --  -48.45-125.00 -60.00   31
 17  \w   -161.00 -74.00   1.00    5.50    --  -86.25 -29.00 -17.00   87
 18  \w   -109.00 -13.00   1.00    5.50    --  -86.25  77.00 120.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0753968000
_diffrn_orient_matrix_UB_12      -0.1181053000
_diffrn_orient_matrix_UB_13      -0.0159891000
_diffrn_orient_matrix_UB_21      0.1048334000
_diffrn_orient_matrix_UB_22      -0.0626509000
_diffrn_orient_matrix_UB_23      -0.0327039000
_diffrn_orient_matrix_UB_31      0.0371458000
_diffrn_orient_matrix_UB_32      0.0096002000
_diffrn_orient_matrix_UB_33      0.0902080000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5478
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22282
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.604
_diffrn_reflns_theta_max         67.604
_diffrn_reflns_theta_min         3.845
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.19a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         7966
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0576P)^2^+1.6219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6409
_reflns_number_total             7966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07276a2.cif
_cod_data_source_block           klb-gr-2
_cod_depositor_comments
'Adding full bibliography for 7127711--7127713.cif.'
_cod_original_cell_volume        2271.64(13)
_cod_database_code               7127711
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNBHBr
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.785
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N1-H1A
 0.9 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C20(H20)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1A), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C27(H27),
 C28(H28), C29(H29), C33(H33), C35(H35), C42(H42), C44(H44), C50(H50), C51(H51),
  C52(H52), C53(H53), C54(H54)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C55(H55A,H55B,H55C)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              82156
_shelx_hkl_checksum              13180
_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 1.491
_oxdiff_exptl_absorpt_empirical_full_min 0.680