Phospholyl(borane) amino acids and peptides: Stereoselective synthesis and fluorescent properties with large Stokes shift.
Arribat, Mathieu; Rémond, Emmanuelle; Clément, Sébastien; Lee, Arie Van Der; Cavelier, Florine; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10954

data_4127005
_publ_section_title
;
 Phospholyl(borane) amino acids and peptides: Stereoselective synthesis
 and fluorescent properties with large Stokes shift.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10954
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H31 B N O4 P'
_chemical_formula_sum            'C24 H31 B N O4 P'
_chemical_formula_weight         439.28
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
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_cell_length_a                   9.58533(17)
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_cell_length_c                   19.2463(3)
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    175
_cell_measurement_theta_max      67.6390
_cell_measurement_theta_min      4.0460
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0143
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -42.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000   60.0000 77

  2 omega   68.00   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.6315  179.0000   30.0000 26

  3 omega   61.00  101.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.6315  179.0000  -90.0000 40

  4 omega   64.00  124.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  179.0000  -30.0000 60

  5 omega  102.00  131.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  112.0000  -30.0000 29

  6 omega  126.00  165.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  112.0000   90.0000 39

  7 omega   59.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -30.0000  120.0000 26

  8 omega   35.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -61.0000  -30.0000 78

  9 omega   56.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -30.0000  -60.0000 34

 10 omega   30.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000 -112.0000 -150.0000 85

 11 omega   62.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  179.0000 -150.0000 86

 12 omega -102.00   -9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -19.0000 -120.0000 93

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0840234000
_diffrn_orient_matrix_UB_12      0.0742485000
_diffrn_orient_matrix_UB_13      -0.0454573000
_diffrn_orient_matrix_UB_21      0.1012520000
_diffrn_orient_matrix_UB_22      0.0864513000
_diffrn_orient_matrix_UB_23      0.0196204000
_diffrn_orient_matrix_UB_31      0.0923840000
_diffrn_orient_matrix_UB_32      -0.0267176000
_diffrn_orient_matrix_UB_33      -0.0628136000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7749
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         67.762
_diffrn_reflns_theta_min         4.068
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details 'Flack (1983), 1838 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     None
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_refine_ls_number_reflns         4068
_refine_ls_number_restraints     3
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_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.0002851
_refine_ls_shift/su_mean         0.0000231
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 17.1 -4.15 13.5 0.328 
;
_refine_ls_weighting_scheme      calc
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_reflns_limit_h_min              -11
_reflns_limit_k_max              15
_reflns_limit_k_min              0
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_reflns_limit_l_min              0
_reflns_number_gt                4068
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_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0552
_oxford_refine_ls_scale          6.075(13)
_oxford_reflns_number_all        4330
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ja7b10954_si_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        2429.30(4)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4127005
_cell_oxdiff_length_a            9.5825(6)
_cell_oxdiff_length_b            13.1617(8)
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_cell_oxdiff_angle_alpha         89.996(5)
_cell_oxdiff_angle_beta          90.015(5)
_cell_oxdiff_angle_gamma         90.141(5)
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