Formation of macrocyclic ring systems by carbonylation of trifunctional P/B/B frustrated Lewis pairs.
Wang, Long; Dong, Shunxi; Daniliuc, Constantin G.; Liu, Lei; Grimme, Stefan; Knitsch, Robert; Eckert, Hellmut; Hansen, Michael Ryan; Kehr, Gerald; Erker, Gerhard; Chemical science 9 (2018) 1544–1550; doi:10.1039/c7sc04394e

data_1548463
_publ_section_title
;
 Formation of macrocyclic ring systems by carbonylation of trifunctional
 P/B/B frustrated Lewis pairs.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              1544
_journal_page_last               1550
_journal_paper_doi               10.1039/c7sc04394e
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C34 H38 B F10 P'
_chemical_formula_weight         678.42
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-05-12 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                102.465(2)
_cell_angle_beta                 96.491(2)
_cell_angle_gamma                91.561(2)
_cell_formula_units_Z            4
_cell_length_a                   13.2091(5)
_cell_length_b                   14.4202(6)
_cell_length_c                   17.4143(7)
_cell_measurement_reflns_used    6443
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     3213.5(2)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.097
_diffrn_reflns_av_sigmaI/netI    0.1013
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22688
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.9967
_exptl_absorpt_correction_T_min  0.9514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         10899
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.1963
_refine_ls_R_factor_gt           0.1255
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+22.5694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2056
_refine_ls_wR_factor_ref         0.2457
_reflns_number_gt                6769
_reflns_number_total             10899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc04394e2.cif
_cod_data_source_block           erk8518
_cod_depositor_comments
'Adding full bibliography for 1548459--1548464.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1548463