#------------------------------------------------------------------------------
#$Date: 2022-04-04 00:52:00 +0300 (Mon, 04 Apr 2022) $
#$Revision: 274284 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/40/4004077.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_4004077
loop_
_publ_author_name
'Xue, Jie'
'Wang, Ziyu'
'Comstock, Andrew'
'Wang, Zhiyu'
'Sung, Herman H. Y.'
'Williams, Ian D.'
'Sun, Dali'
'Liu, Junwei'
'Lu, Haipeng'
_publ_section_title
;
 Chemical Control of Magnetic Ordering in Hybrid Fe--Cl Layered Double
 Perovskites
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2813
_journal_page_last               2823
_journal_paper_doi               10.1021/acs.chemmater.2c00163
_journal_volume                  34
_journal_year                    2022
_chemical_formula_moiety         'Ag Cl8 In, 2(C4 H14 N2)'
_chemical_formula_sum            'C8 H28 Ag Cl8 In N4'
_chemical_formula_weight         686.63
_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             2021-09-07
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_cell_angle_alpha                102.735(7)
_cell_angle_beta                 91.155(6)
_cell_angle_gamma                90.898(6)
_cell_formula_units_Z            1
_cell_length_a                   7.7161(5)
_cell_length_b                   7.8117(7)
_cell_length_c                   9.3428(7)
_cell_measurement_reflns_used    2396
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.1980
_cell_measurement_theta_min      4.8290
_cell_volume                     549.06(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1788
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     82.00 108.00   1.00   16.00    --  113.00-111.00   0.00   26
  2  ω    -73.00  35.00   1.00    8.00    --  -40.20  77.00 120.00  108
  3  ω    -62.00  34.00   1.00    8.00    --  -40.20  57.00   0.00   96
  4  ω     52.00  87.00   1.00    8.00    --   40.20-125.00   0.00   35
  5  ω     13.00 111.00   1.00    8.00    --   40.20  57.00-120.00   98
  6  ω     50.00 138.00   1.00   16.00    --  113.00 -61.00 -30.00   88
  7  ω     43.00  78.00   1.00   16.00    --  113.00-111.00   0.00   35
  8  ω    105.00 177.00   1.00   16.00    --  113.00  77.00 -30.00   72
  9  ω    111.00 161.00   1.00   16.00    --  113.00  77.00-180.00   50
 10  ω    104.00 178.00   1.00   16.00    --  113.00  77.00  60.00   74
 11  ω     35.00 108.00   1.00   16.00    --  113.00-111.00 -90.00   73
 12  ω     35.00 107.00   1.00   16.00    --  113.00-111.00-180.00   72
 13  ω     87.00 178.00   1.00   16.00    --  113.00  61.00 120.00   91
 14  ω    105.00 145.00   1.00   16.00    --  113.00  77.00  30.00   40
 15  ω    148.00 174.00   1.00   16.00    --  113.00  77.00  30.00   26
 16  ω     79.00 112.00   1.00   16.00    --  113.00-126.00 119.00   33
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0702436000
_diffrn_orient_matrix_UB_12      0.0490213000
_diffrn_orient_matrix_UB_13      0.1566353000
_diffrn_orient_matrix_UB_21      -0.1867098000
_diffrn_orient_matrix_UB_22      -0.0332652000
_diffrn_orient_matrix_UB_23      -0.0626955000
_diffrn_orient_matrix_UB_31      0.0100124000
_diffrn_orient_matrix_UB_32      -0.1933667000
_diffrn_orient_matrix_UB_33      0.0114192000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3286
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.182
_diffrn_reflns_theta_min         4.854
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    24.505
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_description       block
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.172
_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     105
_refine_ls_number_reflns         2200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0311
_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)+(0.0710P)²+0.9200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2083
_reflns_number_total             2200
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm2c00163_si_003.cif
_cod_data_source_block           xuejie25cu_173k_auto
_cod_database_code               4004077
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'In Fe Cl4 C4N2H14'
_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   0.527
_shelx_estimated_absorpt_t_min   0.441
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C1(H1D,H1E), C2(H2D,H2E)
2.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.236
_oxdiff_exptl_absorpt_empirical_full_min 0.799
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
In1 In 0.5000 0.5000 0.0000 0.01057(14) Uani 1 2 d S . P . .
Ag1 Ag 0.0000 0.0000 0.0000 0.02665(16) Uani 1 2 d S . P . .
Cl1 Cl 0.74845(13) 0.30529(14) 0.04266(12) 0.0248(2) Uani 1 1 d . . . . .
Cl2 Cl 0.43325(13) 0.55037(14) 0.27012(11) 0.0251(2) Uani 1 1 d . . . . .
Cl3 Cl 0.29806(13) 0.23446(14) -0.04840(12) 0.0250(2) Uani 1 1 d . . . . .
Cl4 Cl 0.05330(14) 0.04105(14) 0.26521(11) 0.0256(2) Uani 1 1 d . . . . .
N2 N 0.0203(5) 0.6104(6) 0.2394(5) 0.0284(9) Uani 1 1 d . . . . .
H2A H 0.1305 0.5862 0.2640 0.034 Uiso 1 1 calc R U . . .
H2B H 0.0221 0.7047 0.1970 0.034 Uiso 1 1 calc R U . . .
H2C H -0.0270 0.5158 0.1749 0.034 Uiso 1 1 calc R U . . .
C3 C -0.0844(5) 0.5063(7) 0.4581(5) 0.0268(9) Uani 1 1 d . . . . .
H3A H -0.1081 0.3927 0.3885 0.032 Uiso 1 1 calc R U . . .
H3B H -0.1800 0.5260 0.5286 0.032 Uiso 1 1 calc R U . . .
C4 C -0.0853(7) 0.6504(6) 0.3736(5) 0.0283(10) Uani 1 1 d . . . . .
H4A H -0.2064 0.6701 0.3451 0.034 Uiso 1 1 calc R U . . .
H4B H -0.0403 0.7604 0.4386 0.034 Uiso 1 1 calc R U . . .
N1 N 0.4576(5) 0.0771(6) 0.2310(5) 0.0281(9) Uani 1 1 d . . . . .
H1A H 0.4996 -0.0241 0.1762 0.034 Uiso 1 1 calc R U . . .
H1B H 0.4534 0.1598 0.1761 0.034 Uiso 1 1 calc R U . . .
H1C H 0.3490 0.0565 0.2605 0.034 Uiso 1 1 calc R U . . .
C1 C 0.5735(6) 0.1409(6) 0.3623(5) 0.0271(9) Uani 1 1 d . . . . .
H1D H 0.5297 0.2533 0.4195 0.033 Uiso 1 1 calc R U . . .
H1E H 0.6912 0.1635 0.3296 0.033 Uiso 1 1 calc R U . . .
C2 C 0.5841(5) 0.0103(6) 0.4604(5) 0.0240(9) Uani 1 1 d . . . . .
H2D H 0.6785 0.0483 0.5345 0.029 Uiso 1 1 calc R U . . .
H2E H 0.6148 -0.1056 0.4000 0.029 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
Cl1 In1 Cl1 180.0 . 2_665 ?
Cl2 In1 Cl1 91.02(3) 2_665 . ?
Cl2 In1 Cl1 88.99(3) . . ?
Cl2 In1 Cl1 88.98(3) 2_665 2_665 ?
Cl2 In1 Cl1 91.02(3) . 2_665 ?
Cl2 In1 Cl2 180.00(5) 2_665 . ?
Cl3 In1 Cl1 89.35(3) 2_665 2_665 ?
Cl3 In1 Cl1 89.35(3) . . ?
Cl3 In1 Cl1 90.65(4) 2_665 . ?
Cl3 In1 Cl1 90.65(3) . 2_665 ?
Cl3 In1 Cl2 89.05(4) 2_665 2_665 ?
Cl3 In1 Cl2 90.95(4) 2_665 . ?
Cl3 In1 Cl2 89.05(4) . . ?
Cl3 In1 Cl2 90.95(4) . 2_665 ?
Cl3 In1 Cl3 180.0 . 2_665 ?
Cl1 Ag1 Cl1 180.00(3) 2_655 1_455 ?
Cl3 Ag1 Cl1 91.65(3) 2 2_655 ?
Cl3 Ag1 Cl1 91.65(3) . 1_455 ?
Cl3 Ag1 Cl1 88.35(3) 2 1_455 ?
Cl3 Ag1 Cl1 88.35(3) . 2_655 ?
Cl3 Ag1 Cl3 180.0 2 . ?
Cl4 Ag1 Cl1 87.80(3) . 2_655 ?
Cl4 Ag1 Cl1 92.20(3) . 1_455 ?
Cl4 Ag1 Cl1 92.20(3) 2 2_655 ?
Cl4 Ag1 Cl1 87.80(3) 2 1_455 ?
Cl4 Ag1 Cl3 84.65(3) 2 . ?
Cl4 Ag1 Cl3 95.35(3) 2 2 ?
Cl4 Ag1 Cl3 95.34(3) . . ?
Cl4 Ag1 Cl3 84.66(3) . 2 ?
Cl4 Ag1 Cl4 180.0 . 2 ?
In1 Cl1 Ag1 161.40(4) . 1_655 ?
In1 Cl3 Ag1 157.92(5) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
C3 C3 H3A 108.6 2_566 . ?
C3 C3 H3B 108.6 2_566 . ?
H3A C3 H3B 107.6 . . ?
C4 C3 C3 114.5(5) . 2_566 ?
C4 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
N2 C4 C3 113.3(4) . . ?
N2 C4 H4A 108.9 . . ?
N2 C4 H4B 108.9 . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N1 C1 H1D 109.1 . . ?
N1 C1 H1E 109.1 . . ?
N1 C1 C2 112.3(4) . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 H1D 109.1 . . ?
C2 C1 H1E 109.1 . . ?
C1 C2 C2 113.8(5) . 2_656 ?
C1 C2 H2D 108.8 . . ?
C1 C2 H2E 108.8 . . ?
C2 C2 H2D 108.8 2_656 . ?
C2 C2 H2E 108.8 2_656 . ?
H2D C2 H2E 107.7 . . ?
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
In1 Cl1 2.5447(10) . ?
In1 Cl1 2.5447(10) 2_665 ?
In1 Cl2 2.5317(10) 2_665 ?
In1 Cl2 2.5318(10) . ?
In1 Cl3 2.5282(10) . ?
In1 Cl3 2.5282(10) 2_665 ?
Ag1 Cl1 3.0612(10) 2_655 ?
Ag1 Cl1 3.0612(10) 1_455 ?
Ag1 Cl3 3.0205(10) . ?
Ag1 Cl3 3.0205(10) 2 ?
Ag1 Cl4 2.4528(10) . ?
Ag1 Cl4 2.4528(10) 2 ?
Cl1 Ag1 3.0612(10) 1_655 ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N2 C4 1.487(6) . ?
C3 C3 1.523(9) 2_566 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.510(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.492(6) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.516(6) . ?
C2 C2 1.531(8) 2_656 ?
C2 H2D 0.9900 . ?
C2 H2E 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C3 C4 N2 73.6(7) 2_566 . . . ?
N1 C1 C2 C2 -69.1(6) . . . 2_656 ?
