Synthesis and reactivity of N,N'-1,4-diazabutadiene derived borocations.
Lawson, James R.; Wilkins, Lewis C.; André, Manon; Richards, Emma C.; Ali, Mohammed N.; Platts, James A.; Melen, Rebecca L.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16177–16181; doi:10.1039/c6dt03360a

data_7040766
_publ_section_title
;
 Synthesis and reactivity of N,N'-1,4-diazabutadiene derived borocations.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16177
_journal_page_last               16181
_journal_paper_doi               10.1039/c6dt03360a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C32 H41 B Cl1 N2, Al Cl4'
_chemical_formula_sum            'C32 H41 Al B Cl5 N2'
_chemical_formula_weight         668.71
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-08-14 deposited with the CCDC.
2016-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9942(4)
_cell_length_b                   18.2174(4)
_cell_length_c                   10.5733(2)
_cell_measurement_reflns_used    22889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0240
_cell_measurement_theta_min      2.2130
_cell_volume                     3658.63(13)
_computing_cell_refinement
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_molecular_graphics    'XSHELL and Mercury'
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            41108
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.418
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.88232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 2388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.025(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0448P)^2^+1.2807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5852
_reflns_number_total             6461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03360a2.cif
_cod_data_source_block           2016ncs0437_sq
_cod_depositor_comments
'Adding full bibliography for 7040765--7040767.cif.'
_cod_database_code               7040766
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2013-3
_shelx_res_checksum              37066
_shelx_fab_checksum              6777