Accurate H-atom parameters for the two polymorphs of <small>L</small>-histidine at 5, 105 and 295K
Novelli, Giulia; McMonagle, Charles J.; Kleemiss, Florian; Probert, Michael; Puschmann, Horst; Grabowsky, Simon; Maynard-Casely, Helen E.; McIntyre, Garry J.; Parsons, Simon; Acta Crystallographica Section B 77 (2021) –; doi:10.1107/S205252062100740X

data_2108886
_publ_section_title
;
 Accurate H-atom parameters for the two polymorphs of
 <small>L</small>-histidine at 5, 105 and 295K
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205252062100740X
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C6 H9 N3 O2'
_chemical_formula_sum            'C6 H9 N3 O2'
_chemical_formula_weight         155.157
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_audit_creation_date             2021-01-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.1521(1)
_cell_length_b                   7.2228(2)
_cell_length_c                   18.8440(6)
_cell_measurement_reflns_used    6123
_cell_measurement_temperature    105
_cell_measurement_theta_max      36.01
_cell_measurement_theta_min      3.02
_cell_volume                     701.23(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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_temperature      105
_diffrn_measured_fraction_theta_full 0.9578
_diffrn_measured_fraction_theta_max 0.8496
_diffrn_measurement_device       'XIPHOS four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.9578
_diffrn_reflns_Laue_measured_fraction_max 0.8496
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13793
_diffrn_reflns_point_group_measured_fraction_full 0.9686
_diffrn_reflns_point_group_measured_fraction_max 0.8648
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         36.32
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'rotating anode'
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker TXS with Helios Optics'
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       needle
_exptl_crystal_F_000             328.072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.1671
_refine_diff_density_min         -0.1507
_refine_diff_density_rms         0.0390
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.4(8)
_refine_ls_d_res_high            0.5999
_refine_ls_d_res_low             6.7443
_refine_ls_goodness_of_fit_ref   1.1223
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2942
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.1027
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0119P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0375
_reflns_Friedel_coverage         0.886
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              28
_reflns_limit_l_min              -28
_reflns_number_gt                2706
_reflns_number_total             2942
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            um5050sup1.cif
_cod_data_source_block           HOTX22
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               2108886
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 H5, H3, H6, C4, N2, C5, N3, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H1A, H1B, H1C, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H3A, C3, H3B, C2, H2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108886