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_7127713
_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         'C18 H B F15 O, C59 H71 B2 N4'
_chemical_formula_sum            'C77 H72 B3 F15 N4 O'
_chemical_formula_weight         1386.81
_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   mixed
_atom_sites_solution_primary     iterative
_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                81.940(3)
_cell_angle_beta                 77.947(3)
_cell_angle_gamma                88.914(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1752(4)
_cell_length_b                   14.7860(5)
_cell_length_c                   21.3743(7)
_cell_measurement_reflns_used    18789
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.1670
_cell_measurement_theta_min      3.9010
_cell_volume                     3419.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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    -68.00  17.00   1.00    0.10    --  -48.45  97.00  95.00   85
  2  \w     -5.00  21.00   1.00    0.10    --   48.45 -97.00 -12.00   26
  3  \w     22.00  55.00   1.00    0.10    --   48.45 -97.00 -12.00   33
  4  \w    -82.00 -48.00   1.00    0.68    --  -86.25  97.00  95.00   34
  5  \w   -155.00 -82.00   1.00    0.68    --  -86.25 -97.00 -12.00   73
  6  \w     40.00  95.00   1.00    0.68    --  106.49 -97.00 -12.00   55
  7  \w   -118.00 -70.00   1.00    0.10    --  -48.45-125.00 150.00   48
  8  \w   -119.00 -72.00   1.00    0.10    --  -48.45-125.00  60.00   47
  9  \w    -63.00  24.00   1.00    0.10    --  -48.45  57.00  60.00   87
 10  \w    -24.00  61.00   1.00    0.10    --   48.45 -38.00-120.00   85
 11  \w    -99.00 -14.00   1.00    0.68    --  -86.25  38.00-120.00   85
 12  \w   -146.00 -84.00   1.00    0.68    --  -86.25 -99.00 -60.00   62
 13  \w     35.00 128.00   1.00    0.68    --  106.49 -77.00  60.00   93
 14  \w     92.00 175.00   1.00    0.68    --  106.49 125.00 -30.00   83
 15  \w     34.00 117.00   1.00    0.68    --  106.49-125.00 -60.00   83
 16  \w     37.00 109.00   1.00    0.68    --  106.49 -99.00  60.00   72
 17  \w     32.00 118.00   1.00    0.68    --  106.49 -19.00 -60.00   86
 18  \w     34.00 109.00   1.00    0.68    --  106.49 -99.00 -60.00   75
 19  \w     99.00 176.00   1.00    0.68    --  106.49  38.00-180.00   77
 20  \w     88.00 178.00   1.00    0.68    --  106.49  77.00-120.00   90
 21  \w    104.00 162.00   1.00    0.68    --  106.49  97.00  95.00   58
;
_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      -0.0183500000
_diffrn_orient_matrix_UB_12      0.0790210000
_diffrn_orient_matrix_UB_13      -0.0522080000
_diffrn_orient_matrix_UB_21      -0.0081678000
_diffrn_orient_matrix_UB_22      -0.0690967000
_diffrn_orient_matrix_UB_23      -0.0466449000
_diffrn_orient_matrix_UB_31      -0.1395325000
_diffrn_orient_matrix_UB_32      -0.0074819000
_diffrn_orient_matrix_UB_33      0.0252556000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33871
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (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    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         12111
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0513P)^2^+1.7177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10129
_reflns_number_total             12111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07276a2.cif
_cod_data_source_block           klb-gr-3
_cod_depositor_comments
'Adding full bibliography for 7127711--7127713.cif.'
_cod_database_code               7127713
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         BCNOF
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.659
_reflns_odcompleteness_completeness 99.16
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1
 0.9 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C35(H35), C52(H52), C55(H55)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C20(H20),
 C27(H27), C28(H28), C29(H29), C33(H33), C42(H42), C44(H44)
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), C53(H53a,H53b,H53c), C54(H54a,H54b,H54c), C56(H56a,H56b,
 H56c), C57(H57a,H57b,H57c), C58(H58a,H58b,H58c), C59(H59a,H59b,H59c)
;
_shelx_res_checksum              17516
_shelx_hkl_checksum              33005
_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 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.522