Selective biocatalytic synthesis and crystal structure of (2R,6R)-hydroxyketaminium chloride, C13H17Cl2NO2
Luelf, U. Joost; Reiss, Guido J.; Bokel, Ansgar; Urlacher, Vlada B.; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 827–829; doi:10.1515/ncrs-2021-0055

data_8104725
_publ_section_title
;
 Selective biocatalytic synthesis and crystal structure of
 (2R,6R)-hydroxyketaminium chloride, C13H17Cl2NO2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              827
_journal_page_last               829
_journal_paper_doi               10.1515/ncrs-2021-0055
_journal_volume                  236
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C13 H17 Cl N O2, Cl'
_chemical_formula_sum            'C13 H17 Cl2 N O2'
_chemical_formula_weight         290.17
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                81.085(3)
_cell_angle_beta                 77.487(4)
_cell_angle_gamma                73.335(4)
_cell_formula_units_Z            2
_cell_length_a                   7.1486(3)
_cell_length_b                   7.8265(3)
_cell_length_c                   13.6579(5)
_cell_measurement_reflns_used    4458
_cell_measurement_temperature    290(1)
_cell_measurement_theta_max      25.4910
_cell_measurement_theta_min      3.5870
_cell_volume                     711.13(5)
_computing_cell_refinement
'CrysAlisPro(Rigaku Oxford Diffraction, 2019)'
_computing_data_collection
'CrysAlisPro(Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction
'CrysAlisPro(Rigaku Oxford Diffraction, 2019)'
_computing_molecular_graphics    'Diamond 4 (Crystal Impact, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      290(1)
_diffrn_detector_area_resol_mean 16.2678
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23627
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         30.814
_diffrn_reflns_theta_min         3.263
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       needle
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.515
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1973 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         8214
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0100P)^2^+0.2754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.897
_reflns_number_gt                5570
_reflns_number_total             8214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0055_suppl.cif
_cod_data_source_block           exp_1460_luelf2_RT2_a
_cod_database_code               8104725
_oxdiff_exptl_absorpt_empirical_full_min 0.813
_oxdiff_exptl_absorpt_empirical_full_max 1.185
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
Absorption correction using spherical harmonics
Frame scaling
;