#------------------------------------------------------------------------------
#$Date: 2022-09-13 01:54:00 +0300 (Tue, 13 Sep 2022) $
#$Revision: 277780 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/12/7711224.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_7711224
loop_
_publ_author_name
'Bruns, Jörn'
'Höppe, Henning A.'
'Hämmer, Matthias'
'Pasqualini, Leonard C.'
'Huppertz, Hubert'
'Sebastian, Sean'
_publ_section_title
;
 Cd[B2(SO4)4] and H2[B2(SO4)4] -- A phyllosilicate analogue borosulfate
 and its homeotypic heteropolyacid
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02344J
_journal_year                    2022
_chemical_formula_moiety         'C2 H8 Ag N2 O4 Re'
_chemical_formula_sum            'C2 H8 Ag N2 O4 Re'
_chemical_formula_weight         418.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2022-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-02 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                117.306(3)
_cell_angle_beta                 115.322(3)
_cell_angle_gamma                93.114(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4566(7)
_cell_length_b                   8.1260(6)
_cell_length_c                   8.1597(7)
_cell_measurement_reflns_used    7726
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      3.02
_cell_volume                     377.30(6)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9866
_diffrn_measured_fraction_theta_max 0.9866
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8593
_diffrn_reflns_theta_full        26.0666
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         2.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.583
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0739 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.8712.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.6806
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.5651
_refine_diff_density_min         -0.8434
_refine_diff_density_rms         0.1774
_refine_ls_d_res_high            0.8087
_refine_ls_d_res_low             6.8603
_refine_ls_goodness_of_fit_ref   1.0692
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0692
_refine_ls_R_factor_all          0.0155
_refine_ls_R_factor_gt           0.0151
_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/[σ²(Fo²)+(0.0132P)²+0.6927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0348
_refine_ls_wR_factor_ref         0.0350
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -9
_reflns_limit_k_max              8
_reflns_limit_k_min              -10
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                1448
_reflns_number_total             1472
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt02344j2.cif
_cod_data_source_block           Ag[C2N2H4][ReO4]
_cod_database_code               7711224
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -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_refinement_flags_posn
Re1 Re 0.25696(2) 0.34094(2) 0.50570(2) 0.00916(6) Uani 1.000000 .
Ag1 Ag 0.65756(4) 0.10481(4) 0.75647(4) 0.01187(8) Uani 1.000000 .
O3 O 0.2372(5) 0.5722(4) 0.6228(5) 0.0189(6) Uani 1.000000 .
O1 O 0.1315(4) 0.1951(4) 0.5518(4) 0.0156(6) Uani 1.000000 .
O2 O 0.5182(5) 0.3551(4) 0.6163(5) 0.0198(6) Uani 1.000000 .
N1 N 0.9648(5) 0.2332(5) 0.8376(6) 0.0112(6) Uani 1.000000 .
N2 N 0.3826(5) -0.0247(5) 0.7308(5) 0.0118(6) Uani 1.000000 .
O4 O 0.1462(5) 0.2345(4) 0.2329(5) 0.0203(6) Uani 1.000000 .
C2 C 0.4046(6) 0.0215(6) 0.9380(6) 0.0114(7) Uani 1.000000 .
C1 C 1.0240(6) 0.4423(6) 0.9122(6) 0.0109(7) Uani 1.000000 .
H7 H 1.157(7) 0.491(6) 0.952(7) 0.002(9) Uiso 1.000000 .
H8 H 0.943(8) 0.455(7) 0.783(8) 0.016(12) Uiso 1.000000 .
H3 H 0.273(9) 0.024(8) 0.667(9) 0.031(15) Uiso 1.000000 .
H6 H 0.990(7) 0.175(7) 0.737(8) 0.012(11) Uiso 1.000000 .
H2 H 0.415(8) 0.158(8) 1.013(8) 0.023(13) Uiso 1.000000 .
H1 H 0.274(8) -0.059(7) 0.908(8) 0.021(12) Uiso 1.000000 .
H4 H 0.340(7) -0.158(8) 0.645(8) 0.014(11) Uiso 1.000000 .
H5 H 1.031(7) 0.216(6) 0.937(8) 0.008(11) Uiso 1.000000 .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
O1 Re1 O3 110.42(13) . . ?
O2 Re1 O3 109.05(14) . . ?
O2 Re1 O1 108.82(13) . . ?
O4 Re1 O3 110.88(14) . . ?
O4 Re1 O1 108.64(14) . . ?
O4 Re1 O2 108.99(15) . . ?
N2 Ag1 N1 168.79(13) . . ?
C1 N1 Ag1 116.7(2) . . ?
H6 N1 Ag1 114(3) . . ?
H6 N1 C1 106(3) . . ?
H5 N1 Ag1 97(3) . . ?
H5 N1 C1 111(3) . . ?
H5 N1 H6 111(4) . . ?
C2 N2 Ag1 114.6(2) . . ?
H3 N2 Ag1 108(3) . . ?
H3 N2 C2 108(3) . . ?
H4 N2 Ag1 111(3) . . ?
H4 N2 C2 106(3) . . ?
H4 N2 H3 109(4) . . ?
C2 C2 N2 110.3(4) 2_657 . ?
H2 C2 N2 106(3) . . ?
H1 C2 N2 109(3) . . ?
H1 C2 H2 109(4) . . ?
C1 C1 N1 109.7(4) 2_767 . ?
H7 C1 N1 113(3) . . ?
H8 C1 N1 108(3) . . ?
H8 C1 H7 102(4) . . ?
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
Re1 O3 1.723(3) . ?
Re1 O1 1.735(3) . ?
Re1 O2 1.732(3) . ?
Re1 O4 1.723(3) . ?
Ag1 Ag1 3.2484(6) 2_656 ?
Ag1 N1 2.141(3) . ?
Ag1 N2 2.134(3) . ?
N1 C1 1.481(5) . ?
N1 H6 0.85(5) . ?
N1 H5 0.83(5) . ?
N2 C2 1.483(5) . ?
N2 H3 0.98(6) . ?
N2 H4 0.92(5) . ?
C2 C2 1.522(8) 2_657 ?
C2 H2 0.97(5) . ?
C2 H1 1.01(5) . ?
C1 C1 1.518(7) 2_767 ?
C1 H7 0.90(4) . ?
C1 H8 1.03(5) . ?
