1,3,2,5-Diazadiborinine featuring nucleophilic and electrophilic boron centres
Di Wu; Lingbing Kong; Yongxin Li; Rakesh Ganguly; Rei Kinjo; Nature Communications 6 (2015) 7340–; doi:10.1038/ncomms8340

data_1548265
_publ_section_title
;
 1,3,2,5-Diazadiborinine featuring nucleophilic and electrophilic boron
 centres
;
_journal_name_full               'Nature Communications'
_journal_page_first              7340
_journal_paper_doi               10.1038/ncomms8340
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C22 H26 B2 Cl2 N2 O2, 0.5(C6 H6)'
_chemical_formula_sum            'C25 H29 B2 Cl2 N2 O2'
_chemical_formula_weight         482.02
_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
_cell_angle_alpha                82.773(9)
_cell_angle_beta                 76.229(9)
_cell_angle_gamma                74.293(9)
_cell_formula_units_Z            2
_cell_length_a                   9.205(3)
_cell_length_b                   10.740(3)
_cell_length_c                   13.922(4)
_cell_measurement_temperature    296(2)
_cell_volume                     1284.1(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15505
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.127
_diffrn_reflns_theta_min         2.353
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.277
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         4454
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.0630
_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^)+(0.1173P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.2137
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2265
_reflns_number_total             4454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms8340-s2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1284.2(6)
_cod_database_code               1548265
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.936
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C11-O1 \\sim C11-O1A \\sim C12-O2 \\sim C12-O2A
 with sigma of 0.02
 N1-C8 \\sim N1-C8A \\sim N2-C14 \\sim N2-C14A
 with sigma of 0.02
3. Rigid bond restraints
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim O1A \\sim C7A \\sim C8A \\sim C9A
\\sim C10A \\sim O2 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim O2A \\sim
C13A \\sim C14A \\sim C15A \\sim C16A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
C21 \\sim C22: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
5. Same fragment restrains
{O1, C7, C8, C9, C10} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1A, C7A, C8A, C9A, C10A}
{O2, C13, C14, C15, C16} sigma for 1-2: 0.02, 1-3: 0.04
as
{O2A, C13A, C14A, C15A, C16A}
6. Others
 Sof(O1A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(O1)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(O2A)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(C15A)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(2)
 Sof(O2)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(2)
 Fixed Sof: C23(0.5) H23(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) C26(0.5)
 H26(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C10A(H10C,H10D), C13(H13A,H13B), C13A(H13C,H13D)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
7.c Fitted hexagon refined as free rotating group:
 C23(C24,C25,C26,C27,C28)
7.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C7A(H7AA,H7AB,H7AC), C9A(H9AA,H9AB,H9AC),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C15A(H15D,H15E,H15F), C16A(H16D,H16E,
 H16F)
;
_shelx_res_checksum              53125
_shelx_hkl_checksum              24523
_olex2_submission_special_instructions 'No special instructions were received'