Indirect synthesis of a pair of formal methane activation products at a phosphane/borane frustrated Lewis pair.
Frömel, Silke; Daniliuc, Constantin G.; Bannwarth, Christoph; Grimme, Stefan; Bussmann, Kathrin; Kehr, Gerald; Erker, Gerhard; Dalton transactions (Cambridge, England : 2003) 45 (2016) 19230–19233; doi:10.1039/c6dt04206f

data_7041185
_publ_section_title
;
 Indirect synthesis of a pair of formal methane activation products at a
 phosphane/borane frustrated Lewis pair.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19230
_journal_page_last               19233
_journal_paper_doi               10.1039/c6dt04206f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C33 H29 B F10 I P'
_chemical_formula_weight         784.24
_space_group_IT_number           2
_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
;
2016-08-24 deposited with the CCDC.
2016-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                87.146(3)
_cell_angle_beta                 83.941(2)
_cell_angle_gamma                64.082(4)
_cell_formula_units_Z            2
_cell_length_a                   10.7065(2)
_cell_length_b                   11.5683(8)
_cell_length_c                   16.2976(5)
_cell_measurement_reflns_used    5473
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     1805.37(15)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20891
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         4.61
_exptl_absorpt_coefficient_mu    8.041
_exptl_absorpt_correction_T_max  0.6029
_exptl_absorpt_correction_T_min  0.1548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+1.4957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                5917
_reflns_number_total             6100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt04206f2.cif
_cod_data_source_block           erk6754
_cod_depositor_comments
'Adding full bibliography for 7041185--7041187.cif.'
_cod_original_cell_volume        1805.37(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7041185