Piezoactive amino acid derivatives containing fragments of planar-chiral ortho-carboranes
Gruzdev, Dmitry A.; Nuraeva, Alla S.; Slepukhin, Pavel A.; Levit, Galina L.; Zelenovskiy, Pavel S.; Shur, Vladimir Ya.; Krasnov, Victor P.; Journal of Materials Chemistry C 6 (2018) 8638–; doi:10.1039/C8TC02266F

data_7237351
_publ_section_title
;
 Piezoactive amino acid derivatives containing fragments of planar-chiral
 ortho-carboranes
;
_journal_issue                   32
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              8638
_journal_paper_doi               10.1039/C8TC02266F
_journal_volume                  6
_journal_year                    2018
_chemical_absolute_configuration (S,S)
_chemical_formula_moiety         'C18 H32 B10 N2 O4'
_chemical_formula_sum            'C18 H32 B10 N2 O4'
_chemical_formula_weight         448.71
_chemical_melting_point          420.5(15)
_chemical_name_systematic
;
(S,S)-tert-Butyl N-(3-formamido-1,2-dicarba-closo-dodecaboran-1-yl)acetylphenylalaninate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2bc 2'
_space_group_name_H-M_alt        'P 2 21 21'
_symmetry_Int_Tables_number      18
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-04-23 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.376(3)
_cell_length_b                   11.388(3)
_cell_length_c                   31.773(17)
_cell_measurement_reflns_used    826
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      66.8322
_cell_measurement_theta_min      2.7836
_cell_volume                     2668.9(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.9539
_diffrn_measured_fraction_theta_max 0.9378
_diffrn_measurement_device_type  'Xcalibur 3'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10617
_diffrn_reflns_theta_full        66.0000
_diffrn_reflns_theta_max         68.14
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  1.12533
_exptl_absorpt_correction_T_min  0.87777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             943.8276
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH-H2O'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.2474
_refine_diff_density_min         -0.3234
_refine_diff_density_rms         0.0544
_refine_ls_d_res_high            0.8307
_refine_ls_d_res_low             15.8866
_refine_ls_goodness_of_fit_ref   1.0372
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    56
_refine_ls_number_parameters     309
_refine_ls_number_reflns         2637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0372
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                1134
_reflns_number_total             2637
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8tc02266f2.cif
_cod_data_source_block           DC1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '419-422 K' was changed to
'420.5(15)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2669(2)
_cod_original_sg_symbol_Hall     ' P 2 2ab (z,x,y)'
_cod_database_code               7237351
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C3(H3a,H3b)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C7(H7), C6(H6a), C5(H5), C14(H14), N0aa(H0aa), N1(H1)
2.d Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C16(H16a,H16b,H16c)
2.e Boron cage BH refined with riding coordinates:
 B9(H9a), B10(H10a), B7(H7a), B8(H8a), B5(H5a), B6(H6), B3(H3), B2(H2a),
 B4(H4), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'