Borane-induced ring closure reaction of oligomethylene-linked bis-allenes
Tao, Xin; Škoch, Karel; Daniliuc, Constantin G.; Kehr, Gerald; Erker, Gerhard; Chemical Science 11 (2020) 1542–1548; doi:10.1039/C9SC03870A

data_1556651
_publ_section_title
;
 Borane-induced ring closure reaction of oligomethylene-linked bis-allenes
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              1542
_journal_page_last               1548
_journal_paper_doi               10.1039/C9SC03870A
_journal_volume                  11
_journal_year                    2020
_chemical_formula_sum            'C46 H38 B Cl2 F10 P'
_chemical_formula_weight         893.44
_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_method           'APEX3 v2016.1-0'
_audit_update_record
;
2019-06-13 deposited with the CCDC.	2019-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                96.789(6)
_cell_angle_beta                 96.943(7)
_cell_angle_gamma                106.576(7)
_cell_formula_units_Z            2
_cell_length_a                   11.1982(12)
_cell_length_b                   11.5411(13)
_cell_length_c                   16.5533(16)
_cell_measurement_reflns_used    3179
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      66.5372
_cell_measurement_theta_min      4.0490
_cell_volume                     2009.0(4)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'APEX3 v2016.1-0 (Bruker AXS Inc., 2016)'
_computing_publication_material  'APEX3 v2016.1-0 (Bruker AXS Inc., 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Kappa CCD APEXII'
_diffrn_measurement_method       'phi / omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24246
_diffrn_reflns_theta_full        67.21
_diffrn_reflns_theta_max         67.21
_diffrn_reflns_theta_min         4.05
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.543
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/5, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.520
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         6850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0730P)^2^+0.6795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1685
_reflns_number_gt                4461
_reflns_number_total             6850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03870a2.cif
_cod_data_source_block           erk9509
_cod_depositor_comments
;Adding full bibliography for 1556647--1556655.cif.

 Adding full bibliography for 1556647--1556655.cif.
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_cod_database_code               1556651
_shelx_res_checksum              88422