Stabilising fleeting intermediates of stilbene photocyclization with amino-borane functionalisation: the rare isolation of persistent dihydrophenanthrenes and their [1,5] H-shift isomers.
Shi, Yong-Gang; Mellerup, Soren K.; Yuan, Kang; Hu, Guo-Fei; Sauriol, Francoise; Peng, Tai; Wang, Nan; Chen, Pangkuan; Wang, Suning; Chemical science 9 (2018) 3844–3855; doi:10.1039/c8sc00560e

data_1549143
_publ_section_title
;
 Stabilising fleeting intermediates of stilbene photocyclization with
 amino-borane functionalisation: the rare isolation of persistent
 dihydrophenanthrenes and their [1,5] H-shift isomers.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              3844
_journal_page_last               3855
_journal_paper_doi               10.1039/c8sc00560e
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C34 H39 B N2'
_chemical_formula_weight         486.50
_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-08 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                66.239(11)
_cell_angle_beta                 88.621(11)
_cell_angle_gamma                75.243(12)
_cell_formula_units_Z            2
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_cell_length_b                   11.896(4)
_cell_length_c                   13.128(5)
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_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.55
_cell_volume                     1417.2(8)
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_number            19796
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_exptl_absorpt_coefficient_mu    0.065
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_description       Block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.180
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_exptl_crystal_size_min          0.095
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_refine_ls_extinction_coef       0.089(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0671
_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^)+(0.1071P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.2045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3597
_reflns_number_total             6268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00560e2.cif
_cod_data_source_block           sy2c
_cod_depositor_comments
;

2019-03-17
Changing obviously wrong Z value and formula.                 miguel

 Adding full bibliography for 1549141--1549152.cif.
;
_cod_original_formula_sum        'C2.43 H2.79 B0.07 N0.14'
_cod_original_formula_units_Z    28
_cod_original_formula_weight     34.75
_cod_database_code               1549143
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              25840