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_7701621
_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     direct
_audit_creation_date             2018-12-24
_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                 94.560(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8544(8)
_cell_length_b                   11.6106(7)
_cell_length_c                   18.2019(9)
_cell_measurement_reflns_used    7066
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.9210
_cell_measurement_theta_min      3.2750
_cell_volume                     2918.7(3)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 10.3385
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.871
_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    -61.00  23.00   1.00   32.00    --   -9.42 -77.00 120.00   84
  2  \w     -7.00  74.00   1.00   32.00    --   11.14  38.00 -90.00   81
  3  \w     26.00  52.00   1.00   32.00    --   11.14 -99.00  90.00   26
  4  \w     35.00  80.00   1.00   32.00    --   11.14 178.00  90.00   45
;
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18817
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.529
_diffrn_reflns_theta_min         2.849
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81258
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.141
_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         0.314
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7088
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0579P)^2^+1.4005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5500
_reflns_number_total             7088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01555h2.cif
_cod_data_source_block           jsc18007
_cod_database_code               7701621
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6BA-H6BA \\sim C6BA-H6BD
 with sigma of 0.02
 C6BA-H6BB \\sim C6BA-H6BF
 with sigma of 0.02
 C6BA-H6BC \\sim C6BA-H6BE
 with sigma of 0.02
 C8CA-H8CA \\sim C8CA-H8CF
 with sigma of 0.02
 C8CA-H8CB \\sim C8CA-H8CD
 with sigma of 0.02
 C8CA-H8CC \\sim C8CA-H8CE
 with sigma of 0.02
 C2DA-H2DA \\sim C2DA-H2DD
 with sigma of 0.02
 C2DA-H2DB \\sim C2DA-H2DE
 with sigma of 0.02
 C2DA-H2DC \\sim C2DA-H2DF
 with sigma of 0.02
3. Others
 Sof(H6BD)=Sof(H6BE)=Sof(H6BF)=1-FVAR(1)
 Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=FVAR(1)
 Sof(H8CD)=Sof(H8CE)=Sof(H8CF)=1-FVAR(2)
 Sof(H8CA)=Sof(H8CB)=Sof(H8CC)=FVAR(2)
 Sof(H2DD)=Sof(H2DE)=Sof(H2DF)=1-FVAR(3)
 Sof(H2DA)=Sof(H2DB)=Sof(H2DC)=FVAR(3)
4.a Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C6AA(H6AA), C3BA(H3BA), C4BA(H4BA), C7BA(H7BA), C0CA(H0CA),
 C1CA(H1CA), C3CA(H3CA), C5CA(H5CA), C7CA(H7CA), C9CA(H9CA), C1DA(H1DA),
 C4DA(H4DA)
4.b Idealised Me refined as rotating group:
 C(HA,HB,HC), C2BA(H2BA,H2BB,H2BC), C6BA(H6BA,H6BB,H6BC), C2CA(H2CA,H2CB,H2CC),
  C4CA(H4CA,H4CB,H4CC), C6CA(H6CA,H6CB,H6CC), C8CA(H8CA,H8CB,H8CC), C2DA(H2DA,
 H2DB,H2DC), C3DA(H3DA,H3DB,H3DC)
;
_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
;