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_7701616
_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         'C28 H18 B F10 N Si'
_chemical_formula_sum            'C28 H18 B F10 N Si'
_chemical_formula_weight         597.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-19
_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                82.624(5)
_cell_angle_beta                 80.864(5)
_cell_angle_gamma                88.285(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7352(5)
_cell_length_b                   10.9636(6)
_cell_length_c                   12.5326(8)
_cell_measurement_reflns_used    5522
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.0000
_cell_measurement_theta_min      3.5210
_cell_volume                     1309.68(13)
_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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3385
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.840
_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  85.00   1.00    8.00    --   11.29  38.00  30.00   97
  2  \w    -13.00  82.00   1.00    8.00    --   11.29  38.00 -60.00   95
  3  \w    -16.00  25.00   1.00    8.00    --   -9.42 -99.00  90.00   41
  4  \w    -16.00  38.00   1.00    8.00    --   11.29 -57.00  30.00   54
  5  \w     35.00  79.00   1.00    8.00    --   11.29-178.00-120.00   44
  6  \w    -36.00   5.00   1.00    8.00    --   -9.42  77.00 120.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0075737000
_diffrn_orient_matrix_UB_12      -0.0329488000
_diffrn_orient_matrix_UB_13      -0.0438324000
_diffrn_orient_matrix_UB_21      -0.0542746000
_diffrn_orient_matrix_UB_22      0.0408018000
_diffrn_orient_matrix_UB_23      -0.0135797000
_diffrn_orient_matrix_UB_31      0.0494291000
_diffrn_orient_matrix_UB_32      0.0388033000
_diffrn_orient_matrix_UB_33      -0.0351099000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13815
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.602
_diffrn_reflns_theta_min         2.815
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88364
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0349P)^2^+0.6077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4701
_reflns_number_total             6195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01555h2.cif
_cod_data_source_block           jsc17116
_cod_original_cell_volume        1309.67(13)
_cod_database_code               7701616
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C28 H18 B F10 N Si'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.962
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_olex2_date_sample_data_collection 2018-10-04
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.452
_oxdiff_exptl_absorpt_empirical_full_min 0.687