Nitro-redox reactions at a frustrated borane/phosphane Lewis pair.
Chen, Guo-Qiang; Kehr, Gerald; Daniliuc, Constantin G.; Erker, Gerhard; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6820–6823; doi:10.1039/c6dt00857g

data_7038784
_publ_section_title
;
 Nitro-redox reactions at a frustrated borane/phosphane Lewis pair.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6820
_journal_page_last               6823
_journal_paper_doi               10.1039/c6dt00857g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C43 H37 B F10 N O2 P'
_chemical_formula_weight         831.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2016-01-29 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.746(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2252(8)
_cell_length_b                   21.5455(12)
_cell_length_c                   15.6095(10)
_cell_measurement_reflns_used    9649
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      27.3640
_cell_measurement_theta_min      2.4464
_cell_volume                     4412.1(5)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection
;
APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)
;
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            69696
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.45
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.91
_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    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
Two badly disordered dichloromethane molecules were found in the 
asymmetrical unit and could not be satisfactorily refined. The program
SQUEEZE (A. L. Spek J. Appl. Cryst., 2003, 36, 7-13) 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         0.570
_refine_diff_density_min         -0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7780
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0769P)^2^+8.0690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1695
_reflns_number_gt                6088
_reflns_number_total             7780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00857g2.cif
_cod_data_source_block           erk8001
_cod_depositor_comments
'Adding full bibliography for 7038780--7038784.cif.'
_cod_database_code               7038784
_shelx_res_checksum              97772