Expansion of the scope of alkylboryl-bridged N → B-ladder boranes: new substituents and alternative substrates.
Pammer, Frank; Schepper, Jonas; Glöckler, Johannes; Sun, Yu; Orthaber, Andreas; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10298–10312; doi:10.1039/c9dt01555h

data_7701620
_publ_section_title
;
 Expansion of the scope of alkylboryl-bridged N \\rightarrow B-ladder
 boranes: new substituents and alternative substrates.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10298
_journal_page_last               10312
_journal_paper_doi               10.1039/c9dt01555h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H40 B N Si'
_chemical_formula_sum            'C34 H40 B N Si'
_chemical_formula_weight         501.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-27 deposited with the CCDC.	2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.702(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8845(3)
_cell_length_b                   11.7689(3)
_cell_length_c                   20.7907(7)
_cell_measurement_reflns_used    12958
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      28.6920
_cell_measurement_theta_min      3.6010
_cell_volume                     3075.47(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.95(10)
_diffrn_detector_area_resol_mean 10.3385
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  28.00   1.00   64.00    --   -9.42 -99.00  60.00   40
  2  \w      1.00  28.00   1.00   64.00    --   -9.42 -99.00 -60.00   27
  3  \w    -16.00  10.00   1.00   64.00    --   -9.42 -57.00   0.00   26
  4  \w    -17.00  21.00   1.00   64.00    --   -9.42 -99.00 -90.00   38
  5  \w    -62.00  24.00   1.00   64.00    --   11.14 -57.00 -60.00   86
  6  \w     48.00  98.00   1.00   64.00    --   11.14 178.00 -60.00   50
  7  \w     27.00  52.00   1.00   64.00    --   11.14  19.00-150.00   25
  8  \w    -27.00  -1.00   1.00   64.00    --   11.14  19.00-150.00   26
  9  \w    -63.00  36.00   1.00   64.00    --   11.14 -38.00   0.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34861
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.490
_diffrn_reflns_theta_min         2.868
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7717
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.5440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6029
_reflns_number_total             7717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01555h2.cif
_cod_data_source_block           jsc18002
_cod_original_cell_volume        3075.49(16)
_cod_database_code               7701620
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All H(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 Si1-C27A \\sim Si1-C27B
 with sigma of 0.02
 Si1-C28A \\sim Si1-C28B
 with sigma of 0.02
 Si1-C26A \\sim Si1-C26B
 with sigma of 0.02
 C30-H30A \\sim C30-H30D
 with sigma of 0.02
 C30-H30B \\sim C30-H30E
 with sigma of 0.02
 C30-H30C \\sim C30-H30F
 with sigma of 0.02
 C33-H33A \\sim C33-H33E
 with sigma of 0.02
 C33-H33B \\sim C33-H33F
 with sigma of 0.02
 C33-H33C \\sim C33-H33D
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C28A, C27A, C26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si1, C27A, C28A, C26A, C28B, C26B, C27B, H26D, H26E, H26F, H26A, H26B, H26C,
 H28D, H28E, H28F, H28A, H28B, H28C, H27D, H27E, H27F, H27A, H27B, H27C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C26B)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28A)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(2)
 Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(2)
 Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(3)
 Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C18(H18), C2(H2), C1(H1), C7(H7), C22(H22), C4(H4), C16(H16),
 C3(H3), C9(H9), C8(H8), C10(H10)
5.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C27A(H27A,H27B,H27C),
 C28A(H28A,H28B,H28C), C26A(H26A,H26B,H26C), C28B(H28D,H28E,H28F), C26B(H26D,
 H26E,H26F), C27B(H27D,H27E,H27F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;