Innocent BN bond substitution in anthracene derivatives.
van de Wouw, H. L.; Lee, J. Y.; Siegler, M. A.; Klausen, R. S.; Organic & biomolecular chemistry 14 (2016) 3256–3263; doi:10.1039/c5ob02309b

data_7154985
_publ_section_title
;
 Innocent BN bond substitution in anthracene derivatives.
;
_journal_issue                   12
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3256
_journal_page_last               3263
_journal_paper_doi               10.1039/c5ob02309b
_journal_volume                  14
_journal_year                    2016
_chemical_formula_moiety         'C19 H16 B N'
_chemical_formula_sum            'C19 H16 B N'
_chemical_formula_weight         269.14
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-11-05 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                94.271(4)
_cell_angle_beta                 91.188(4)
_cell_angle_gamma                90.053(3)
_cell_formula_units_Z            4
_cell_length_a                   5.9219(3)
_cell_length_b                   7.4968(3)
_cell_length_c                   31.3180(19)
_cell_measurement_reflns_used    5546
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      67.20
_cell_measurement_theta_min      4.22
_cell_volume                     1386.21(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            15319
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.250
_diffrn_reflns_theta_min         4.248
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1458P)^2^+0.4587P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2349
_refine_ls_wR_factor_ref         0.2466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4038
_reflns_number_total             5846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ob02309b2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7154985--7154990.cif.'
_cod_database_code               7154985
_twin_information
;
 * * * CRYSALIS TWIN DATA REDUCTION FINALIZING (Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)) * * *
Laue class: 1bar - Friedel mate is equivalent
Lattice type: P-lattice 
DC PROFFITRRPTWIN INFO: Step 1 - Loading orientation matrices (UB) of 2 components
 
DC PROFFITRRPTWIN INFO: Loading UB component 1
 
DC PROFFITRRPTWIN INFO: Loading UB component 2
 
DC PROFFITRRPTWIN INFO: Step 2 - Computing crossed twin laws
 
Twin law determination (relative to component 1)
Matrix 1 is taken from component 1 (   5.920    7.495   31.311    94.30    91.14    90.11)
Matrix 2 is taken from component 2 (   5.915    7.489   31.311    93.98    90.97    89.90)
Twin analysis: Component 1 with component 2
TL  =UB[1]-1*UB[2]:  -1.0007  -0.0002  -0.0001    -0.0003   1.0007  -0.0001     0.0184  -0.6046  -0.9995   det 1.001002
TL-1=UB[2]*UB[1]-1:  -0.9993  -0.0002   0.0001    -0.0003   0.9992  -0.0001    -0.0183  -0.6045  -1.0004   det 0.998999
Rot= -179.8008 deg around the following vectors: 
Reciprocal space (hkl): -0.0015 0.9573 -0.2892
Direct space (uvw)    : -0.0001 1.0000 0.0006
 
DC PROFFITRRPTWIN INFO: Step 3 - Loading reflections of 2 components
 
DC PROFFITRRPTWIN ALL INFO: Component 1
DC PROFFITRRPTWIN INFO: Face list of component 1 
  1:   0.0035  -0.0009  19.9929  d=   0.0172
  2:   2.9997  -3.0006   5.7474  d=   0.0984
  3:  -1.0029   4.0005 -14.3809  d=   0.0794
  4:   2.9949   1.9999 -13.2507  d=   0.0886
  5:   0.0034  -3.0004  14.7976  d=   0.0833
  6:  -0.0035   0.0009 -19.9929  d=   0.0010
  7:   1.0007   2.9989  13.1746  d=   0.0987
  8:  -3.9975   2.0006   0.8690  d=   0.1149
  9:  -1.9953  -2.0001  15.2321  d=   0.0914
 10:   1.0010  -4.9986  -1.9999  d=   0.1063
 11:  -1.0008  -1.9966 -16.7848  d=   0.0513
DC PROFFITRRPTWIN ALL INFO: Component 2
DC PROFFITRRPTWIN INFO: Face list of component 2 
  1:  -0.0024  -0.0025 -20.0010  d=   0.0172
  2:  -2.9967  -2.9995  -3.9909  d=   0.0984
  3:   1.0006   3.9988  11.9873  d=   0.0794
  4:  -2.9939   1.9986  11.9928  d=   0.0886
  5:  -0.0020  -2.9993 -12.9905  d=   0.0833
  6:   0.0024   0.0025  20.0010  d=   0.0010
  7:  -0.9999   2.9953 -15.0113  d=   0.0987
  8:   3.9943   2.0000  -2.0056  d=   0.1149
  9:   1.9951  -1.9993 -13.9933  d=   0.0914
 10:  -0.9994  -4.9948   5.0039  d=   0.1063
 11:   0.9996  -1.9934  18.0172  d=   0.0513
 
DC PROFFITRRPTWIN INFO: Step 4 - Analysing composite reflections of 2 components
 
Component 1: 18001 observations read
Component 2: 17996 observations read

21109 composite observations collected (6261 fully isolated, 14848 overlapped), 29 skipped due to one or more missing parts and 4 skipped due to I/sig<-3.0

OVERLAP STATISTICS

2 COMPONENTS

COMPONENTS 1, 2
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |       3421 |    16.2 <--- ALMOST SEPARATED
   0.20 - 0.40  |       2910 |    13.8
   0.40 - 0.60  |       3023 |    14.3
   0.60 - 0.80  |       3323 |    15.7
   0.80 - 1.00  |       2171 |    10.3 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |      14848 |    70.3

 
DC PROFFITRRPTWIN INFO: Step 5 - Scaling data & analysing twin ratios of 2 components
 
Computed twin ratios:
Twin 1: 72.75% (9206 common observations, 2384 merged)
Twin 2: 27.25% (7326 common observations, 2384 merged)

Preparing data for SCALE3 ABSPACK...

SCALING COMPONENT 1

10161 of 17976 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-762287.1875 max=10095266.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=107.3130 max=61827.7813
PROFFIT INFO: 93 observations on 'bad frames' rejected

SCALING COMPONENT 2

9382 of 17981 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-2648298.2500 max=10095266.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=101.4021 max=61827.7813
PROFFIT INFO: 125 observations on 'bad frames' rejected

Computed twin ratios:
Twin 1: 72.83% (9172 common observations, 2383 merged)
Twin 2: 27.17% (7311 common observations, 2383 merged)

DC PROFFITRRPTWIN INFO: Determining HKLF4 overlap threshold for completeness requirement (>=80.0%)
DC PROFFITRRPTWIN INFO: New HKLF4 overlap threshold - 0.53

DC PROFFITRRPTWIN INFO: Step 6 - Decomposed intensities statistics (HKLF4)
 
COMPONENT 1

 
Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only!
    Mean F2 and F2/sig(F2) are given for all measured values!
Note: The RsigmaA values are computed for all measured values!

Help: For more information about computations of rint and rsigma please look into Crysalis help: 
 file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html
 

Statistics vs intensity - point group symmetry: P-1
         intensity measured   kept    unique  redundancy   F2     F2/sig(F2)   Rint   Rsigma
  9581023-   96768     1695     1695      398    4.3    467174.98   101.41    0.078    0.099
    95828-   38553     1347     1347      398    3.4     60527.07    35.65    0.118    0.129
    38459-   19319     1400     1400      398    3.5     27786.21    20.41    0.128    0.155
    19295-   10838     1174     1174      398    2.9     14388.64    12.34    0.139    0.154
    10815-    6204     1153     1153      398    2.9      8393.15     7.87    0.165    0.178
     6189-    3623     1164     1164      398    2.9      4770.39     4.72    0.233    0.272
     3619-    2037     1081     1081      398    2.7      2780.91     2.81    0.284    0.320
     2035-    1024     1050     1050      398    2.6      1498.57     1.57    0.414    0.456
     1024-     295     1119     1119      398    2.8       645.36     0.71    0.648    0.841
      291-   -6088      956      956      400    2.4      -119.94    -0.09    0.971    2.121
  9581023-   -6088    12139    12139     3982    3.0     78227.34    23.31    0.088    0.112
 

Statistics vs resolution - point group symmetry: P-1
resolu-      #        #        #               average    mean      mean          
tion(A)   measured   kept    unique           redundancy   F2     F2/sig(F2)   Rint   Rsigma   RsigmaA
 inf-1.85     2871     2871      398             7.2    211828.54    51.13    0.083    0.115     0.010
1.85-1.48     2273     2273      398             5.7     61769.57    20.57    0.081    0.094     0.028
1.48-1.31     1720     1720      398             4.3     26949.04     9.59    0.139    0.167     0.061
1.30-1.17     1211     1211      398             3.0     48005.57    14.89    0.110    0.119     0.038
1.17-1.07      766      766      398             1.9     54441.11    22.97    0.075    0.080     0.028
1.07-1.00      683      683      398             1.7     24247.11    13.73    0.092    0.094     0.053
1.00-0.95      720      720      398             1.8     17742.49    10.74    0.119    0.131     0.066
0.95-0.91      664      664      398             1.7     16810.94    11.77    0.108    0.107     0.064
0.91-0.87      629      629      398             1.6     13026.45     9.86    0.110    0.111     0.073
0.87-0.84      602      602      400             1.5     10231.31    10.22    0.117    0.118     0.078
 inf-0.84    12139    12139     3982             3.0     78227.34    23.31    0.088    0.112     0.020
 

Statistics vs resolution (taking redundancy into account) - point group symmetry: P-1
resolu-      #        #        #       %       average    mean      mean          
tion(A)    kept     theory   unique complete  redundancy   F2     F2/sig(F2)   Rint  RsigmaB
 inf-1.85     2871      455      398   87.5      7.2    211828.54   140.15    0.083    0.004
1.85-1.48     2273      423      398   94.1      5.7     61769.57    51.45    0.081    0.012
1.48-1.31     1720      441      398   90.2      4.3     26949.04    21.40    0.139    0.033
1.30-1.17     1211      490      398   81.2      3.0     48005.57    28.94    0.110    0.021
1.17-1.07      766      525      398   75.8      1.9     54441.11    36.00    0.075    0.019
1.07-1.00      683      528      398   75.4      1.7     24247.11    19.10    0.092    0.035
1.00-0.95      720      496      398   80.2      1.8     17742.49    15.69    0.119    0.049
0.95-0.91      664      555      398   71.7      1.7     16810.94    15.49    0.108    0.049
0.91-0.87      629      530      398   75.1      1.6     13026.45    12.87    0.110    0.055
0.87-0.84      602      521      400   76.8      1.5     10231.31    13.13    0.117    0.058
 inf-0.84    12139     4964     3982   80.2      3.0     78227.34    55.14    0.088    0.013
DC PROFFITRRPTWIN INFO: Step 7 - Generating output files
 
HKLF 4
Reflections read=17882, from those 12139 with overlapping factor < 0.526 written to file C:\Users\msiegle2\Desktop\xs0463a_2\xs0463a_max2_twin1_hklf4.hkl, 5743 skipped
Use the HKLF 4 file(s) for structure solution.

HKLF 5 merged
RINT ANALYSIS FOR ALL HKLF5 REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
1,2          17882     15319      5853     2.62     21.79     0.032     0.033

RINT ANALYSIS FOR OVERLAPPED REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
1,2          14702     12588      4610     2.73     21.19     0.034     0.034

RINT ANALYSIS FOR ISOLATED REFLECTIONS
 Component measured     kept     unique redundancy F2/sig(F2) Rint      Rsigma
     1        3180      2731      1243     2.20     24.57     0.023     0.027
     2           0         0         0     0.00      0.00     0.000     0.000

5853 merged reflections saved into file: C:\Users\msiegle2\Desktop\xs0463a_2\xs0463a_max2_twin1_hklf5.hkl

Use this hkl file in SHELXL with BASF instruction, which has (components minus 1) entries, and HKLF 5 instruction.
E.g. Two component twin: 'BASF n2' in .ins file, BASF n1 can be computed as n1 = 1.0 - n2.
E.g. Three component twin: 'BASF n2 n3' in .ins file, BASF n1 can be computed as n1 = 1.0 - (n2 + n3).

BASF 0.27173 
;
_shelxl_version_number           2013-2
_shelx_res_checksum              89630
_shelx_hkl_checksum              6676