#------------------------------------------------------------------------------
#$Date: 2020-08-06 16:00:44 +0300 (Thu, 06 Aug 2020) $
#$Revision: 254897 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/67/7126742.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7126742
loop_
_publ_author_name
'Ward, Jas S.'
'Fiorini, Giorgia'
'Frontera, Antonio'
'Rissanen, Kari'
_publ_section_title
;
 Asymmetric [N-I-N]⁺ halonium complexes.
;
_journal_issue                   60
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8428
_journal_page_last               8431
_journal_paper_doi               10.1039/d0cc02758h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C14 H20 Ag N4, F6 P'
_chemical_formula_sum            'C14 H20 Ag F6 N4 P'
_chemical_formula_weight         497.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-15 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.059(7)
_cell_angle_beta                 109.119(6)
_cell_angle_gamma                113.062(7)
_cell_formula_units_Z            2
_cell_length_a                   8.6651(13)
_cell_length_b                   10.6439(13)
_cell_length_c                   11.5780(16)
_cell_measurement_reflns_used    1917
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.407
_cell_volume                     918.0(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      170
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5083
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0919 before and 0.0646 after correction. The Ratio of minimum to maximum transmission is 0.6291. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0628
_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/[σ²(Fo²)+(0.0237P)²+4.4488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2686
_reflns_number_total             3723
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc02758h2.cif
_cod_data_source_block           1b_2
_cod_depositor_comments
'Adding full bibliography for 7126741--7126748.cif.'
_cod_database_code               7126742
_shelxl_version_number           2014/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.586
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C22(H22), C23(H23), C25(H25), C26(H26)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.0000 1.0000 0.5000 0.0513(2) Uani 1 2 d S T P . .
Ag2 Ag 0.5000 1.0000 0.5000 0.0566(2) Uani 1 2 d S T P . .
P31 P -0.0415(2) 0.67953(18) 0.26926(17) 0.0485(4) Uani 1 1 d . . . . .
F32 F 0.0701(8) 0.6965(7) 0.1843(5) 0.121(2) Uani 1 1 d . . . . .
F33 F 0.1338(6) 0.7883(4) 0.3756(4) 0.0704(13) Uani 1 1 d . . . . .
F34 F -0.1480(8) 0.6751(7) 0.3557(6) 0.126(2) Uani 1 1 d . . . . .
F35 F -0.0852(7) 0.8033(5) 0.2146(5) 0.108(2) Uani 1 1 d . . . . .
F36 F -0.2159(6) 0.5739(5) 0.1655(5) 0.0946(18) Uani 1 1 d . . . . .
F37 F 0.0037(8) 0.5598(5) 0.3247(6) 0.113(2) Uani 1 1 d . . . . .
N1 N 0.1923(7) 0.9551(5) 0.6391(5) 0.0452(13) Uani 1 1 d . . . . .
N7 N 0.5754(6) 0.8737(5) 0.9189(5) 0.0435(12) Uani 1 1 d . . . . .
N21 N 0.5766(8) 0.8463(6) 0.5819(5) 0.0506(14) Uani 1 1 d . . . . .
N27 N 0.7274(8) 0.5672(6) 0.7828(6) 0.0611(16) Uani 1 1 d . . . . .
C2 C 0.3496(9) 1.0550(7) 0.7072(7) 0.0496(16) Uani 1 1 d . . . . .
H2 H 0.3719 1.1470 0.6921 0.060 Uiso 1 1 calc R . . . .
C3 C 0.4813(8) 1.0336(6) 0.7975(6) 0.0456(15) Uani 1 1 d . . . . .
H3 H 0.5928 1.1091 0.8405 0.055 Uiso 1 1 calc R . . . .
C4 C 0.4513(8) 0.8990(6) 0.8269(5) 0.0380(13) Uani 1 1 d . . . . .
C5 C 0.2867(8) 0.7942(6) 0.7549(6) 0.0402(14) Uani 1 1 d . . . . .
H5 H 0.2588 0.7013 0.7691 0.048 Uiso 1 1 calc R . . . .
C6 C 0.1651(8) 0.8254(6) 0.6637(6) 0.0416(14) Uani 1 1 d . . . . .
H6 H 0.0553 0.7516 0.6149 0.050 Uiso 1 1 calc R . . . .
C8 C 0.5341(9) 0.7362(7) 0.9531(7) 0.0532(17) Uani 1 1 d . . . . .
H8A H 0.4253 0.7055 0.9738 0.080 Uiso 1 1 calc GR . . . .
H8B H 0.6345 0.7382 1.0249 0.080 Uiso 1 1 calc GR . . . .
H8C H 0.5146 0.6721 0.8837 0.080 Uiso 1 1 calc GR . . . .
C9 C 0.7526(8) 0.9829(7) 0.9862(7) 0.0559(19) Uani 1 1 d . . . . .
H9A H 0.8123 1.0226 0.9279 0.084 Uiso 1 1 calc GR . . . .
H9B H 0.8247 0.9443 1.0463 0.084 Uiso 1 1 calc GR . . . .
H9C H 0.7396 1.0551 1.0297 0.084 Uiso 1 1 calc GR . . . .
C22 C 0.7404(9) 0.8838(8) 0.6673(7) 0.0541(18) Uani 1 1 d . . . . .
H22 H 0.8227 0.9780 0.6818 0.065 Uiso 1 1 calc R . . . .
C23 C 0.7961(9) 0.7943(7) 0.7349(7) 0.0527(17) Uani 1 1 d . . . . .
H23 H 0.9138 0.8267 0.7951 0.063 Uiso 1 1 calc R . . . .
C24 C 0.6789(9) 0.6550(7) 0.7150(6) 0.0479(16) Uani 1 1 d . . . . .
C25 C 0.5066(9) 0.6154(7) 0.6241(6) 0.0481(16) Uani 1 1 d . . . . .
H25 H 0.4216 0.5218 0.6063 0.058 Uiso 1 1 calc R . . . .
C26 C 0.4632(9) 0.7128(7) 0.5621(6) 0.0487(16) Uani 1 1 d . . . . .
H26 H 0.3462 0.6844 0.5017 0.058 Uiso 1 1 calc R . . . .
C28 C 0.6033(11) 0.4216(8) 0.7640(9) 0.078(3) Uani 1 1 d . . . . .
H28A H 0.5008 0.4141 0.7866 0.116 Uiso 1 1 calc GR . . . .
H28B H 0.6654 0.3707 0.8159 0.116 Uiso 1 1 calc GR . . . .
H28C H 0.5607 0.3825 0.6770 0.116 Uiso 1 1 calc GR . . . .
C29 C 0.9012(12) 0.6132(9) 0.8851(8) 0.075(2) Uani 1 1 d . . . . .
H29A H 0.9987 0.6535 0.8529 0.113 Uiso 1 1 calc GR . . . .
H29B H 0.9105 0.5341 0.9252 0.113 Uiso 1 1 calc GR . . . .
H29C H 0.9102 0.6828 0.9455 0.113 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ag1 N1 180.0 2_576 . ?
N21 Ag2 N21 180.0 2_676 . ?
F32 P31 F33 89.5(3) . . ?
F32 P31 F34 175.5(4) . . ?
F32 P31 F35 87.6(4) . . ?
F32 P31 F36 91.3(3) . . ?
F34 P31 F33 87.8(3) . . ?
F34 P31 F35 88.7(4) . . ?
F34 P31 F36 91.3(3) . . ?
F35 P31 F33 89.4(2) . . ?
F36 P31 F33 178.9(3) . . ?
F36 P31 F35 89.9(3) . . ?
F37 P31 F32 92.5(4) . . ?
F37 P31 F33 89.7(3) . . ?
F37 P31 F34 91.1(4) . . ?
F37 P31 F35 179.1(3) . . ?
F37 P31 F36 91.0(3) . . ?
C2 N1 Ag1 120.9(4) . . ?
C2 N1 C6 116.2(5) . . ?
C6 N1 Ag1 122.9(4) . . ?
C4 N7 C8 120.4(5) . . ?
C4 N7 C9 121.3(5) . . ?
C8 N7 C9 118.3(5) . . ?
C22 N21 Ag2 119.2(5) . . ?
C22 N21 C26 117.2(6) . . ?
C26 N21 Ag2 123.3(5) . . ?
C24 N27 C28 120.8(7) . . ?
C24 N27 C29 121.7(6) . . ?
C28 N27 C29 117.4(6) . . ?
N1 C2 H2 117.9 . . ?
N1 C2 C3 124.2(6) . . ?
C3 C2 H2 117.9 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 119.9(6) . . ?
C4 C3 H3 120.0 . . ?
N7 C4 C3 122.0(5) . . ?
N7 C4 C5 122.2(6) . . ?
C5 C4 C3 115.8(6) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0(6) . . ?
C6 C5 H5 120.0 . . ?
N1 C6 C5 123.9(6) . . ?
N1 C6 H6 118.1 . . ?
C5 C6 H6 118.1 . . ?
N7 C8 H8A 109.5 . . ?
N7 C8 H8B 109.5 . . ?
N7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7 C9 H9A 109.5 . . ?
N7 C9 H9B 109.5 . . ?
N7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N21 C22 H22 118.1 . . ?
N21 C22 C23 123.7(7) . . ?
C23 C22 H22 118.1 . . ?
C22 C23 H23 120.2 . . ?
C22 C23 C24 119.5(7) . . ?
C24 C23 H23 120.2 . . ?
N27 C24 C23 120.7(7) . . ?
N27 C24 C25 122.6(6) . . ?
C23 C24 C25 116.6(6) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 C24 119.4(6) . . ?
C26 C25 H25 120.3 . . ?
N21 C26 C25 123.5(6) . . ?
N21 C26 H26 118.2 . . ?
C25 C26 H26 118.2 . . ?
N27 C28 H28A 109.5 . . ?
N27 C28 H28B 109.5 . . ?
N27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N27 C29 H29A 109.5 . . ?
N27 C29 H29B 109.5 . . ?
N27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N1 2.113(5) 2_576 ?
Ag1 N1 2.113(5) . ?
Ag2 N21 2.111(6) 2_676 ?
Ag2 N21 2.111(6) . ?
P31 F32 1.556(6) . ?
P31 F33 1.599(4) . ?
P31 F34 1.558(6) . ?
P31 F35 1.586(5) . ?
P31 F36 1.571(4) . ?
P31 F37 1.554(5) . ?
N1 C2 1.330(8) . ?
N1 C6 1.354(8) . ?
N7 C4 1.357(7) . ?
N7 C8 1.453(8) . ?
N7 C9 1.460(8) . ?
N21 C22 1.337(9) . ?
N21 C26 1.340(8) . ?
N27 C24 1.326(8) . ?
N27 C28 1.465(9) . ?
N27 C29 1.471(10) . ?
C2 H2 0.9500 . ?
C2 C3 1.367(9) . ?
C3 H3 0.9500 . ?
C3 C4 1.415(8) . ?
C4 C5 1.395(8) . ?
C5 H5 0.9500 . ?
C5 C6 1.371(8) . ?
C6 H6 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.366(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.397(9) . ?
C24 C25 1.411(9) . ?
C25 H25 0.9500 . ?
C25 C26 1.364(9) . ?
C26 H26 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
