Borane-catalysed dinitrogen borylation by 1,3-B-H bond addition.
Coffinet, Anaïs; Zhang, Dan; Vendier, Laure; Bontemps, Sébastien; Simonneau, Antoine; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5582–5589; doi:10.1039/d1dt00317h

data_7706867
_publ_section_title
;
 Borane-catalysed dinitrogen borylation by 1,3-B-H bond addition.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5582
_journal_page_last               5589
_journal_paper_doi               10.1039/d1dt00317h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '2(C40 H64 B2 F10 N2 P4 W), C7 H8'
_chemical_formula_sum            'C87 H136 B4 F20 N4 P8 W2'
_chemical_formula_weight         2276.76
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2021-01-26 deposited with the CCDC.	2021-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.795(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.15760(4)
_cell_length_b                   19.95340(4)
_cell_length_c                   23.90660(4)
_cell_measurement_reflns_used    7059
_cell_measurement_temperature    110
_cell_measurement_theta_max      23.07
_cell_measurement_theta_min      2.50
_cell_volume                     9662.05(16)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.166
_diffrn_reflns_av_unetI/netI     0.224
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77544
_diffrn_reflns_theta_full        25.082
_diffrn_reflns_theta_max         25.082
_diffrn_reflns_theta_min         1.433
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.596
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4616
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.31
_refine_diff_density_min         -1.88
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9265
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         4240
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.0020924
_refine_ls_shift/su_mean         0.0000351
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.524 0.239 0.332 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1072
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0399
_reflns_limit_h_max              24
_reflns_limit_h_min              -25
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                4786
_reflns_number_total             8550
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            d1dt00317h2.cif
_cod_data_source_block           ACN250220
_cod_depositor_comments
'Adding full bibliography for 7706865--7706867.cif.'
_cod_original_cell_volume        9662.06(13)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               7706867