B-B bond activation and NHC ring-expansion reactions of diboron(4) compounds, and accurate molecular structures of B2(NMe2)4, B2eg2, B2neop2 and B2pin2.
Eck, Martin; Würtemberger-Pietsch, Sabrina; Eichhorn, Antonius; Berthel, Johannes H. J.; Bertermann, Rüdiger; Paul, Ursula S. D.; Schneider, Heidi; Friedrich, Alexandra; Kleeberg, Christian; Radius, Udo; Marder, Todd B.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3661–3680; doi:10.1039/c7dt00334j

data_7042154
_publ_section_title
;
 B-B bond activation and NHC ring-expansion reactions of diboron(4)
 compounds, and accurate molecular structures of B2(NMe2)4, B2eg2, B2neop2
 and B2pin2.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3661
_journal_page_last               3680
_journal_paper_doi               10.1039/c7dt00334j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C39 H46 B2 N2 O4, 0.5(C7 H8)'
_chemical_formula_sum            'C42.5 H50 B2 N2 O4'
_chemical_formula_weight         674.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-01-25 deposited with the CCDC.
2017-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.354(4)
_cell_angle_beta                 96.904(4)
_cell_angle_gamma                98.937(4)
_cell_formula_units_Z            4
_cell_length_a                   12.395(2)
_cell_length_b                   14.186(2)
_cell_length_c                   23.450(4)
_cell_measurement_reflns_used    9350
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.0885
_cell_measurement_theta_min      2.284
_cell_volume                     4042.4(11)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_radiation_monochromator  helios
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45950
_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_max         26.097
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_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Sadabs 2014/4 (Bruker 2014)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       block
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         16033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0560
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_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^)+(0.0508P)^2^+1.5916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12724
_reflns_number_total             16033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00334j2.cif
_cod_data_source_block           HS121
_cod_depositor_comments
;
Adding full bibliography for 7042146--7042160.cif.

2017-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        4042.6(11)
_cod_original_formula_moiety     '2(C39 H46 B2 N2 O4), C7 H8'
_cod_original_formula_sum        'C85 H100 B4 N4 O8'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1348.92
_cod_database_code               7042154
_shelxl_version_number           2014/6
_shelx_res_checksum              87847
_shelx_fab_checksum              29342