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_7127712
_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         'C49 H50 B2 N2 O2, C3 H3'
_chemical_formula_sum            'C52 H53 B2 N2 O2'
_chemical_formula_weight         759.58
_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
_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                86.111(4)
_cell_angle_beta                 83.103(3)
_cell_angle_gamma                72.919(4)
_cell_formula_units_Z            2
_cell_length_a                   8.1757(3)
_cell_length_b                   13.4922(6)
_cell_length_c                   19.8843(8)
_cell_measurement_reflns_used    7768
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.1080
_cell_measurement_theta_min      3.4030
_cell_volume                     2080.25(15)
_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      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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     28.00 117.00   1.00    0.90    --   48.45  77.00-120.00   89
  2  \w    111.00 136.00   1.00    5.60    --  106.49 126.00-146.00   25
  3  \w    128.00 177.00   1.00    5.60    --  106.49  77.00-180.00   49
  4  \w     90.00 178.00   1.00    5.60    --  106.49  61.00-150.00   88
  5  \w     84.00 118.00   1.00    5.60    --  106.49  77.00-180.00   34
  6  \w     36.00 113.00   1.00    5.60    --  106.49 -45.00 -90.00   77
  7  \w     42.00  72.00   1.00    0.90    --   48.45-144.00 -31.00   30
  8  \w     49.00 130.00   1.00    5.60    --  106.49-144.00 -31.00   81
  9  \w     59.00  91.00   1.00    0.90    --   48.45-126.00 137.00   32
 10  \w     57.00 118.00   1.00    5.60    --  106.49-126.00 137.00   61
 11  \w     54.00 108.00   1.00    5.60    --  106.49 -94.00 150.00   54
 12  \w     32.00 119.00   1.00    5.60    --  106.49 -30.00  60.00   87
 13  \w     94.00 171.00   1.00    5.60    --  106.49  30.00 150.00   77
 14  \w     80.00 105.00   1.00    5.60    --  106.49 144.00  22.00   25
 15  \w     34.00 123.00   1.00    5.60    --  106.49 -61.00 -90.00   89
 16  \w    -94.00 -44.00   1.00    0.90    --  -48.45 144.00  22.00   50
 17  \w    -91.00 -39.00   1.00    0.90    --  -48.45 126.00-146.00   52
 18  \w    -90.00 -25.00   1.00    5.60    --  -86.25 126.00-146.00   65
 19  \w   -104.00 -24.00   1.00    5.60    --  -86.25 144.00  22.00   80
 20  \w   -156.00 -73.00   1.00    5.60    --  -86.25 -30.00-180.00   83
 21  \w    -95.00 -62.00   1.00    0.90    --  -48.45-144.00 -31.00   33
 22  \w   -109.00 -70.00   1.00    0.90    --  -48.45-126.00 137.00   39
 23  \w   -117.00 -29.00   1.00    0.90    --  -48.45 -77.00 150.00   88
 24  \w   -145.00-120.00   1.00    5.60    --  -86.25-144.00 -31.00   25
 25  \w   -139.00-114.00   1.00    5.60    --  -86.25-126.00 137.00   25
;
_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      -0.0367095000
_diffrn_orient_matrix_UB_12      -0.0078761000
_diffrn_orient_matrix_UB_13      0.0776967000
_diffrn_orient_matrix_UB_21      -0.0483566000
_diffrn_orient_matrix_UB_22      -0.1008940000
_diffrn_orient_matrix_UB_23      -0.0060174000
_diffrn_orient_matrix_UB_31      0.1886963000
_diffrn_orient_matrix_UB_32      -0.0635893000
_diffrn_orient_matrix_UB_33      0.0049575000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19731
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.072
_diffrn_reflns_theta_max         67.072
_diffrn_reflns_theta_min         3.429
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29359
_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    1.213
_exptl_crystal_description       plate
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.058
_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     535
_refine_ls_number_reflns         7330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0743
_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^)+(0.1046P)^2^+1.4880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5854
_reflns_number_total             7330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07276a2.cif
_cod_data_source_block           klb-gr-5
_cod_depositor_comments
'Adding full bibliography for 7127711--7127713.cif.'
_cod_database_code               7127712
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CBNO
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.733
_reflns_odcompleteness_completeness 98.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C29(H29), C48(H48), C11(H11), C38(H38), C12(H12), C36(H36),
 C46(H46), C27(H27), C6(H6), C22(H22), C20(H20), C21(H21), C56(H56), C57(H57),
 C58(H58)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C41(H41A,H41B,H41C), C54(H54A,H54B,
 H54C), C55(H55A,H55B,H55C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C51(H51A,
 H51B,H51C), C31(H31A,H31B,H31C), C52(H52A,H52B,H52C), C50(H50A,H50B,H50C),
 C42(H42A,H42B,H42C)
;
_shelx_res_checksum              74803
_shelx_hkl_checksum              22360
_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 2.635
_oxdiff_exptl_absorpt_empirical_full_min 0.439