Spontaneous N<sub>2</sub>-diboranylation of [W(N<sub>2</sub>)<sub>2</sub>(dppe)<sub>2</sub>] with B<sub>2</sub>Br<sub>4</sub>(SMe<sub>2</sub>)<sub>2</sub>.
Haufe, Lisa C.; Arrowsmith, Merle; Dietz, Maximilian; Gärtner, Annalena; Bertermann, Rüdiger; Braunschweig, Holger; Dalton transactions (Cambridge, England : 2003)  (2022) –; doi:10.1039/d2dt02135h

data_7710783
_publ_section_title
;
 Spontaneous N<sub>2</sub>-diboranylation of
 [W(N<sub>2</sub>)<sub>2</sub>(dppe)<sub>2</sub>] with
 B<sub>2</sub>Br<sub>4</sub>(SMe<sub>2</sub>)<sub>2</sub>.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt02135h
_journal_year                    2022
_chemical_formula_moiety         'C55 H57 B2 Br4 N2 P5 W, 2(C6 H6)'
_chemical_formula_sum            'C67 H69 B2 Br4 N2 P5 W'
_chemical_formula_weight         1582.20
_chemical_name_systematic        1-PMe3
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'CIF-fill 1.2y (K.Radacki, 2005-22)'
_audit_update_record
;
2022-05-18 deposited with the CCDC.	2022-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.100(6)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   19.060(4)
_cell_length_b                   38.289(8)
_cell_length_c                   28.618(8)
_cell_measurement_reflns_used    9168
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      2.67
_cell_volume                     19351(8)
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_collection       'BIS 6.2.14 / APEX3 ver. 2019.1 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPA
_diffrn_detector_area_resol_mean 7.5
_diffrn_detector_type            'Photon II'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            235517
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.349
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.868
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_exptl_absorpt_coefficient_mu    4.435
_exptl_absorpt_correction_T_max  0.6839
_exptl_absorpt_correction_T_min  0.4767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       plate
_exptl_crystal_F_000             9408
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.337
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.498(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2279
_refine_ls_number_reflns         34486
_refine_ls_number_restraints     572
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+27.4966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.985
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                31452
_reflns_number_total             34486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02135h2.cif
_cod_data_source_block           test_a_CCDC4
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               7710783
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.286
_shelx_estimated_absorpt_t_max   0.777
_shelx_res_checksum              38606
_shelx_hkl_checksum              80109