Hydroboration route to geminal P/B frustrated Lewis pairs with a bulky secondary phosphane component and their reaction with carbon dioxide
Erker, Gerhard; Jian, Zhongbao; Kehr, Gerald; Daniliuc, Constantin Gabriel; Wibbeling, Birgit; Dalton Trans.  (2017) –; doi:10.1039/C7DT02315D

data_7043911
_publ_section_title
;
 Hydroboration route to geminal P/B frustrated Lewis pairs with a bulky
 secondary phosphane component and their reaction with carbon dioxide
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02315D
_journal_year                    2017
_chemical_formula_sum            'C73 H80 B2 F20 O2 P2'
_chemical_formula_weight         1452.93
_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   mixed
_audit_update_record
;
2017-07-18 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                102.460(2)
_cell_angle_beta                 90.487(2)
_cell_angle_gamma                117.418(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6152(5)
_cell_length_b                   14.7429(5)
_cell_length_c                   22.6757(7)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      66.7253
_cell_measurement_theta_min      3.4857
_cell_volume                     3914.5(2)
_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    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           ' Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35965
_diffrn_reflns_theta_full        66.93
_diffrn_reflns_theta_max         66.93
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'Cu ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.78
_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    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.103
_platon_squeeze_details
;
Probably two badly disordered dichloromethane molecules were found in the 
asymmetrical unit and could not be satisfactorily refined. The program 
SQUEEZE (Spek, A.L. (2015). Acta Cryst. C71, 9-18) was therefore used to
remove mathematically the effect of the solvent.
The quoted formula and derived parameters are not included the squeezed
solvent molecules.
;
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1294
_refine_ls_number_reflns         12771
_refine_ls_number_restraints     1010
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.1023
_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^)+(0.0240P)^2^+22.7968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2086
_refine_ls_wR_factor_ref         0.2287
_reflns_number_gt                7966
_reflns_number_total             12771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02315d2.cif
_cod_data_source_block           16a
_cod_database_code               7043911
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              79818
_shelx_fab_checksum              15466