UV-mediated anomeric activation.
Fischer, Niklas Henrik; Bałuta, Alicja Klaudia; Szpak, Maciej Tadeusz; Thulstrup, Peter Waaben; Pedersen, Christian Marcus; Organic & biomolecular chemistry 23 (2025) 8928–8936; doi:10.1039/d5ob01184a

data_7160731
_publ_section_title
;
 UV-mediated anomeric activation.
;
_journal_issue                   39
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8928
_journal_page_last               8936
_journal_paper_doi               10.1039/d5ob01184a
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'Cl, C6 H14 N'
_chemical_formula_sum            'C6 H14 Cl N'
_chemical_formula_weight         135.63
_chemical_name_systematic        'Cyclohexylammonium chloride'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-22 deposited with the CCDC.	2025-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.220(3)
_cell_length_b                   11.185(4)
_cell_length_c                   7.437(3)
_cell_measurement_reflns_used    391
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      3.64
_cell_volume                     766.9(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_unetI/netI     0.0944
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6473
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.411
_diffrn_reflns_theta_min         1.821
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6336
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0864 before and 0.0752 after correction.
The Ratio of minimum to maximum transmission is 0.8500.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_F_000             296
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 392 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.10(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1564
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                1153
_reflns_number_total             1564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01184a2.cif
_cod_data_source_block           full
_cod_depositor_comments          'Adding full bibliography for 7160731.cif.'
_cod_database_code               7160731
_shelx_shelxl_version_number     2019/1
_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
2.a Ternary CH refined with riding coordinates:
 C006(H006)
2.b Secondary CH2 refined with riding coordinates:
 C003(H00D,H00E), C004(H00F,H00G), C005(H00H,H00I), C007(H00J,H00K), C008(H00L,
 H00M)
2.c Idealised Me refined as rotating group:
 N002(H00A,H00B,H00C)
;
_shelx_res_checksum              44832
_olex2_submission_special_instructions 'No special instructions were received'