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_1548461
_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            'C31 H32 B F10 P'
_chemical_formula_weight         636.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2017-05-12 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.052(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6792(14)
_cell_length_b                   8.5320(7)
_cell_length_c                   19.5972(15)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      66.5169
_cell_measurement_theta_min      3.1309
_cell_volume                     2919.2(4)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0919
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43312
_diffrn_reflns_theta_full        67.37
_diffrn_reflns_theta_max         67.37
_diffrn_reflns_theta_min         3.67
_diffrn_source                   'fine--focus sealed tube'
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison,
Wisconsin, USA.'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0391P)^2^+2.1996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                3915
_reflns_number_total             5066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04394e2.cif
_cod_data_source_block           erk8657
_cod_depositor_comments
'Adding full bibliography for 1548459--1548464.cif.'
_cod_database_code               1548461
_shelx_res_checksum              31922