Halogenoborane mediated allene cyclooligomerization
Erker, Gerhard; Tao, Xin; Wölke, Christian; Daniliuc, Constantin Gabriel; Kehr, Gerald; Chemical Science  (2019) –; doi:10.1039/C8SC04790A

data_1550428
_publ_section_title
;
 Halogenoborane mediated allene cyclooligomerization
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04790A
_journal_year                    2019
_chemical_formula_sum            'C29 H21 B Cl F10 N'
_chemical_formula_weight         619.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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           'APEX3 v2016.1-0'
_audit_update_record
;
2018-08-17 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                88.589(8)
_cell_angle_beta                 80.364(7)
_cell_angle_gamma                79.511(8)
_cell_formula_units_Z            2
_cell_length_a                   10.2284(12)
_cell_length_b                   11.0264(13)
_cell_length_c                   12.5397(13)
_cell_measurement_reflns_used    2983
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      64.6307
_cell_measurement_theta_min      4.0775
_cell_volume                     1371.0(3)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0958
_diffrn_reflns_av_unetI/netI     0.1026
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20385
_diffrn_reflns_theta_full        66.76
_diffrn_reflns_theta_max         66.76
_diffrn_reflns_theta_min         4.46
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.050
_exptl_absorpt_correction_T_max  0.96
_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    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.255
_refine_ls_extinction_coef       0.0046(6)
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         4780
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0709P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                2842
_reflns_number_total             4780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04790a2.cif
_cod_data_source_block           erk9164
_cod_database_code               1550428
_shelx_res_checksum              11049
_shelx_fab_checksum              46403