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_1549142
_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            'C32 H36 B N S'
_chemical_formula_weight         477.49
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 98.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9250(4)
_cell_length_b                   21.8524(8)
_cell_length_c                   16.0075(6)
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_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.60
_cell_volume                     2739.8(2)
_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            60597
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.130
_diffrn_reflns_theta_min         2.265
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
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_exptl_crystal_description       Block
_exptl_crystal_F_000             1024
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_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         6043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.124
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+2.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2213
_refine_ls_wR_factor_ref         0.2442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4049
_reflns_number_total             6043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00560e2.cif
_cod_data_source_block           sy23
_cod_depositor_comments
;

2019-03-17
Changing absurd Z value and formula.                 miguel

 Adding full bibliography for 1549141--1549152.cif.
;
_cod_original_formula_sum        'C3.66 H4.11 B0.11 N0.11 S0.11'
_cod_original_formula_units_Z    35
_cod_original_formula_weight     54.57
_cod_database_code               1549142
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              60938