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_7701619
_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         'C17 H16 B N3'
_chemical_formula_sum            'C17 H16 B N3'
_chemical_formula_weight         273.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 101.037(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4822(3)
_cell_length_b                   14.3531(5)
_cell_length_c                   11.9681(5)
_cell_measurement_reflns_used    5968
_cell_measurement_temperature    150(10)
_cell_measurement_theta_max      29.3890
_cell_measurement_theta_min      3.7170
_cell_volume                     1430.12(9)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(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 0.908
_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    -10.00  17.00   1.00   24.00    --   -9.42 -99.00  30.00   27
  2  \w     -1.00  25.00   1.00   24.00    --   11.29 -57.00 120.00   26
  3  \w     12.00  37.00   1.00   24.00    --   11.29 -57.00  60.00   25
  4  \w     -7.00  52.00   1.00   24.00    --   11.29 -99.00  30.00   59
  5  \w    -58.00  13.00   1.00   24.00    --   11.29 -38.00 150.00   71
  6  \w    -41.00 -15.00   1.00   24.00    --   11.29 -38.00  60.00   26
  7  \w    -54.00 -18.00   1.00   24.00    --   11.29 -57.00 120.00   36
  8  \w    -17.00  83.00   1.00   24.00    --   11.29  57.00 -90.00  100
;
_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      0.0332428000
_diffrn_orient_matrix_UB_12      0.0198754000
_diffrn_orient_matrix_UB_13      -0.0445958000
_diffrn_orient_matrix_UB_21      -0.0424308000
_diffrn_orient_matrix_UB_22      0.0419518000
_diffrn_orient_matrix_UB_23      0.0047588000
_diffrn_orient_matrix_UB_31      0.0659355000
_diffrn_orient_matrix_UB_32      0.0169744000
_diffrn_orient_matrix_UB_33      0.0404388000
_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     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14563
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.524
_diffrn_reflns_theta_min         2.828
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74372
_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 orangish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       irregular
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3623
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0423P)^2^+0.6458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3020
_reflns_number_total             3623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01555h2.cif
_cod_data_source_block           jsc17108
_cod_original_cell_volume        1430.12(10)
_cod_database_code               7701619
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C17 H16 B N3'
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.986
_reflns_odcompleteness_completeness 99.84
_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. Restrained distances
 C16A-B1 = C17B-B1
 1.55 with sigma of 0.02
 N0AA-B1 = N2B-B1
 1.8 with sigma of 0.02
 N2A-C16A = N3B-C17B
 1.13 with sigma of 0.01
 N2B-C16B = N3B-C17B
 1.13 with sigma of 0.01
 N2B-C16B = N0AA-C17A
 1.14 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C17B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N2B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C16A)=Sof(N2A)=Sof(N0AA)=Sof(C17A)=1-FVAR(1)
 Sof(C17B)=Sof(N3B)=Sof(C16B)=Sof(N2B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C13(H13)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_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 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.805