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_7706865
_publ_section_title
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 Borane-catalysed dinitrogen borylation by 1,3-B-H bond addition.
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_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         'C32 H74 B2 N2 P4 W1'
_chemical_formula_sum            'C32 H74 B2 N2 P4 W'
_chemical_formula_weight         816.32
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
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2021-01-26 deposited with the CCDC.	2021-03-16 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 92.842(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.04190(2)
_cell_length_b                   20.70460(3)
_cell_length_c                   15.84060(3)
_cell_measurement_reflns_used    8921
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.30
_cell_volume                     3944.564(15)
_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      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.138
_diffrn_reflns_av_unetI/netI     0.183
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            113933
_diffrn_reflns_theta_full        27.694
_diffrn_reflns_theta_max         28.260
_diffrn_reflns_theta_min         1.620
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.114
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         4.81
_refine_diff_density_min         -4.00
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6630
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.0024628
_refine_ls_shift/su_mean         0.0000353
_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: 
 0.503 -0.466 0.312 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0312
_refine_ls_wR_factor_gt          0.0247
_refine_ls_wR_factor_ref         0.0238
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                7249
_reflns_number_total             9696
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            d1dt00317h2.cif
_cod_data_source_block           ACN111219
_cod_depositor_comments
'Adding full bibliography for 7706865--7706867.cif.'
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C32 H74 B2 N2 P4 W1'
_cod_database_code               7706865
_publcif_funding_html
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