On pyridine chloronium cations
Pröhm, Patrick; Berg, Willi; Rupf, Susanne Margot; Müller, Carsten; Riedel, Sebastian; Chemical Science 14 (2023) 2325–2329; doi:10.1039/D2SC06757A

data_1568410
_publ_section_title
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 On pyridine chloronium cations
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              2325
_journal_page_last               2329
_journal_paper_doi               10.1039/D2SC06757A
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C20 H20 Ag N4, 2(B F4), 2(C3 H5 N)'
_chemical_formula_sum            'C26 H30 Ag B2 F8 N6'
_chemical_formula_weight         708.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-06
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
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_audit_update_record
;
2022-11-30 deposited with the CCDC.	2023-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6718(18)
_cell_length_b                   15.798(2)
_cell_length_c                   15.142(2)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.38
_cell_volume                     3270.5(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23765
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_min         1.970
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0910 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.7923.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.595
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0321P)^2^+14.3894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3021
_reflns_number_total             3359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06757a2.cif
_cod_data_source_block           pbcn_notwin
_cod_depositor_comments
'Adding full bibliography for 1568406--1568411.cif.'
_cod_original_cell_volume        3270.6(7)
_cod_database_code               1568410
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.805
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C401) = Uanis(C402) = Uanis(C405) = Uanis(C404)
3. Others
 Fixed Sof: C400(0.33333) C401(0.33333) H40F(0.33333) H40G(0.33333)
 C402(0.33333) H40H(0.33333) H40I(0.33333) H40J(0.33333) C403(0.66667)
 C404(0.66667) H40D(0.66667) H40E(0.66667) C405(0.66667) H40A(0.66667)
 H40B(0.66667) H40C(0.66667)
4.a Secondary CH2 refined with riding coordinates:
 C401(H40F,H40G), C404(H40D,H40E)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C30(H30), C31(H31), C32(H32)
4.c Idealised Me refined with everything fixed:
 C402(H40H,H40I,H40J)
4.d Idealised Me refined as rotating group:
 C405(H40A,H40B,H40C)
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_shelx_res_checksum              45852
_shelx_hkl_checksum              60534
_olex2_submission_special_instructions 'No special instructions were received'