A large anisotropic plasticity of <small>L</small>-leucinium hydrogen maleate preserved at cryogenic temperatures
Arkhipov, S. G.; Losev, E. A.; Nguyen, T. T.; Rychkov, D. A.; Boldyreva, E. V.; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619000441

data_2108374
_publ_section_title
;
 A large anisotropic plasticity of <small>L</small>-leucinium hydrogen
 maleate preserved at cryogenic temperatures
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619000441
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_iupac          'C6 H14 N O2 +, C4 H3 O4 -'
_chemical_formula_moiety         'C6 H14 N O2 +, C4 H3 O4 -'
_chemical_formula_sum            'C10 H17 N O6'
_chemical_formula_weight         247.24
_chemical_name_systematic
;
<i>L</i>-Leucinium hydrogen maleate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.653(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   21.4563(9)
_cell_length_b                   5.67251(19)
_cell_length_c                   32.0779(8)
_cell_measurement_reflns_used    4785
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.3540
_cell_measurement_theta_min      2.1340
_cell_volume                     3849.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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    -90.00  90.00   0.50  180.00    --    0.00 180.00 214.00  360
  2  \w    -20.00  90.00   0.50  180.00    --    0.00 180.00 114.00  220
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0162739000
_diffrn_orient_matrix_UB_12      -0.0036395000
_diffrn_orient_matrix_UB_13      -0.0211438000
_diffrn_orient_matrix_UB_21      -0.0291967000
_diffrn_orient_matrix_UB_22      0.0146174000
_diffrn_orient_matrix_UB_23      0.0073259000
_diffrn_orient_matrix_UB_31      0.0029283000
_diffrn_orient_matrix_UB_32      0.1240532000
_diffrn_orient_matrix_UB_33      -0.0014962000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            22918
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.925
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       needle
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          4
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7634
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0494P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.941
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                4962
_reflns_number_total             7634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5052sup1.cif
_cod_data_source_block           l_leu_mal_200
_cod_database_code               2108374
_cod_database_fobs_code          2108374
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C10 H17 N O6'
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.676
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), C22(H22), C43(H43), C41(H41), C23(H23), C42(H42)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C92(H92), C91(H91), C93(H93), C83(H83), C81(H81), C82(H82)
2.d Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N1(H1A,H1B,H1C), C61(H61A,H61B,H61C),
 C63(H63A,H63B,H63C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C62(H62A,H62B,
 H62C), C52(H52A,H52B,H52C)
2.e Idealised tetrahedral OH refined as rotating group:
 O61(H61), O12(H12), O62(H62), O63(H63), O13(H13), O11(H11)
;
_shelx_res_checksum              22778
_shelx_hkl_checksum              99557
_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 1.413
_oxdiff_exptl_absorpt_empirical_full_min 0.792