#------------------------------------------------------------------------------
#$Date: 2019-11-24 09:45:01 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237513 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/72/7237241.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_7237241
loop_
_publ_author_name
'Silva, Ingrid F.'
'Teixeira, Ivo F.'
'Barros, Wdeson P.'
'Pinheiro, Carlos B.'
'Ardisson, José D.'
'do Nascimento, Gustavo M.'
'Pradie, Noriberto A.'
'Teixeira, Ana Paula C.'
'Stumpf, Humberto O.'
_publ_section_title
;
 An FeIII dinuclear metallacycle complex as a size-selective adsorbent for
 nitrogenous compounds and a potentially effective ammonia storage
 material
;
_journal_issue                   25
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              15225
_journal_paper_doi               10.1039/C8TA09786K
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety
'C24 H24 Cl2 Fe2 N4 O14 S2, 2(C2 H6 O S), 2(C H2 Cl2)'
_chemical_formula_sum            'C30 H40 Cl6 Fe2 N4 O16 S4'
_chemical_formula_weight         1165.34
_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_primary     iterative
_audit_creation_date             2018-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-02 deposited with the CCDC.	2019-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                113.668(3)
_cell_angle_beta                 97.457(2)
_cell_angle_gamma                105.922(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3990(3)
_cell_length_b                   10.4057(3)
_cell_length_c                   12.8116(4)
_cell_measurement_reflns_used    18357
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.0270
_cell_measurement_theta_min      1.8001
_cell_volume                     1174.84(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 10.4186
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -76.00   12.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082  -38.0000  -90.0000 88

#__ type_ start__ end____ width___ exp.time_
  2 omega  -41.00   59.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082   38.0000   90.0000 100

#__ type_ start__ end____ width___ exp.time_
  3 omega  -17.00   85.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957   77.0000 -180.0000 102

#__ type_ start__ end____ width___ exp.time_
  4 omega   58.00  107.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957  179.0000    0.0000 49

#__ type_ start__ end____ width___ exp.time_
  5 omega   64.00   90.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957 -153.0000   72.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega -104.00  -32.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082  179.0000  150.0000 72

#__ type_ start__ end____ width___ exp.time_
  7 omega  -93.00   19.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082  -77.0000 -180.0000 112

#__ type_ start__ end____ width___ exp.time_
  8 omega  -91.00   12.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082  -38.0000   30.0000 103

#__ type_ start__ end____ width___ exp.time_
  9 omega  -59.00   28.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957  -38.0000  -30.0000 87

#__ type_ start__ end____ width___ exp.time_
 10 omega   16.00   41.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957 -122.0000 -134.0000 25

#__ type_ start__ end____ width___ exp.time_
 11 omega   16.00   72.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957 -122.0000   52.0000 56

#__ type_ start__ end____ width___ exp.time_
 12 omega  -59.00   28.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957  -38.0000  150.0000 87

#__ type_ start__ end____ width___ exp.time_
 13 omega   56.00  107.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957  179.0000 -120.0000 51
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0719645000
_diffrn_orient_matrix_UB_12      0.0192951000
_diffrn_orient_matrix_UB_13      0.0037629000
_diffrn_orient_matrix_UB_21      0.0159610000
_diffrn_orient_matrix_UB_22      0.0424988000
_diffrn_orient_matrix_UB_23      0.0623635000
_diffrn_orient_matrix_UB_31      -0.0007171000
_diffrn_orient_matrix_UB_32      -0.0646717000
_diffrn_orient_matrix_UB_33      0.0065933000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29473
_diffrn_reflns_theta_full        28.2784
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.6470
_exptl_crystal_description       block
_exptl_crystal_F_000             596.3563
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.8793
_refine_diff_density_min         -1.2749
_refine_diff_density_rms         0.0797
_refine_ls_d_res_high            0.7501
_refine_ls_d_res_low             11.2903
_refine_ls_goodness_of_fit_ref   1.0417
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    31
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0417
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0393P)²+1.3391P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              12
_reflns_limit_k_min              -13
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5317
_reflns_number_total             5826
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ta09786k2.cif
_cod_data_source_block           feopba_re_10
_cod_database_code               7237241
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), N2(H2), N1(H1)
2.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C13(H13a,H13b,H13c), C12(H12a,H12b,H12c), C11(H11a,H11b,
 H11c)
;
_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
Fe1 Fe 0.71897(3) 0.55078(3) 1.33077(2) 0.01468(7) Uani 1.000000 .
S1 S 1.01942(5) 0.76712(5) 1.47964(4) 0.02234(11) Uani 1.000000 .
O1 O 0.51496(13) 0.52199(14) 1.26153(11) 0.0174(2) Uani 1.000000 .
O4 O 0.24442(14) 0.44931(14) 0.82705(11) 0.0185(3) Uani 1.000000 .
O5 O 0.32271(14) 0.66649(14) 0.76909(11) 0.0179(3) Uani 1.000000 .
O7 O 0.92279(14) 0.61003(15) 1.38367(13) 0.0231(3) Uani 1.000000 .
O3 O 0.61396(14) 0.90904(14) 1.36326(12) 0.0215(3) Uani 1.000000 .
O6 O 0.33793(16) 0.83758(15) 0.95169(13) 0.0251(3) Uani 1.000000 .
O2 O 0.73579(13) 0.76675(14) 1.37940(11) 0.0174(2) Uani 1.000000 .
N1 N 0.38288(16) 0.65463(16) 1.23534(13) 0.0159(3) Uani 1.000000 .
N2 N 0.25028(15) 0.61140(16) 1.01283(13) 0.0148(3) Uani 1.000000 .
C2 C 0.19427(17) 0.50424(19) 1.05283(16) 0.0146(3) Uani 1.000000 .
C9 C 0.26635(17) 0.57795(19) 0.90593(16) 0.0151(3) Uani 1.000000 .
C1 C 0.25742(18) 0.52823(19) 1.16526(16) 0.0157(3) Uani 1.000000 .
C7 C 0.49972(18) 0.64235(19) 1.27587(15) 0.0152(3) Uani 1.000000 .
C8 C 0.62669(18) 0.78932(19) 1.34570(15) 0.0160(3) Uani 1.000000 .
C10 C 0.31459(18) 0.7104(2) 0.87677(16) 0.0167(3) Uani 1.000000 .
C11 C 1.1617(3) 0.7324(3) 1.5383(3) 0.0452(7) Uani 1.000000 .
C12 C 1.0916(3) 0.8563(3) 1.3978(3) 0.0518(8) Uani 1.000000 .
Cl1 Cl 0.68318(5) 0.54356(6) 1.49804(4) 0.02518(11) Uani 1.000000 .
S2 S 0.41472(5) 1.03450(5) 1.24136(4) 0.02101(10) Uani 1.000000 .
O8 O 0.30933(15) 0.88354(14) 1.21475(12) 0.0206(3) Uani 1.000000 .
C13 C 0.4471(2) 1.1475(2) 1.39599(19) 0.0283(4) Uani 1.000000 .
C14 C 0.3182(2) 1.1251(2) 1.1905(2) 0.0299(5) Uani 1.000000 .
C4 C 0.01887(19) 0.2790(2) 1.02545(19) 0.0235(4) Uani 1.000000 .
C6 C 0.1997(2) 0.4298(2) 1.20833(18) 0.0221(4) Uani 1.000000 .
C5 C 0.0798(2) 0.3053(2) 1.1385(2) 0.0263(4) Uani 1.000000 .
C3 C 0.07541(18) 0.3781(2) 0.98263(17) 0.0192(3) Uani 1.000000 .
Cl2 Cl 0.38504(7) 0.27396(8) 0.96303(7) 0.04415(16) Uani 1.000000 .
Cl3 Cl 0.13097(9) 0.01803(8) 0.81253(9) 0.0688(3) Uani 1.000000 .
C15 C 0.3135(3) 0.0801(3) 0.8687(2) 0.0393(6) Uani 1.000000 .
H6 H 0.2411(2) 0.4470(2) 1.28389(18) 0.0265(4) Uiso 1.000000 R
H5 H 0.0403(2) 0.2396(2) 1.1676(2) 0.0316(5) Uiso 1.000000 R
H4 H -0.06029(19) 0.1943(2) 0.97817(19) 0.0282(5) Uiso 1.000000 R
H3 H 0.03389(18) 0.3603(2) 0.90693(17) 0.0230(4) Uiso 1.000000 R
H2 H 0.27552(15) 0.70501(16) 1.06218(13) 0.0177(3) Uiso 1.000000 R
H1 H 0.38205(16) 0.74304(16) 1.25185(13) 0.0190(3) Uiso 1.000000 R
H14a H 0.2818(16) 1.0698(11) 1.1059(3) 0.0448(7) Uiso 1.000000 GR
H14b H 0.2428(11) 1.1289(18) 1.2262(12) 0.0448(7) Uiso 1.000000 GR
H14c H 0.3778(5) 1.2255(7) 1.2118(14) 0.0448(7) Uiso 1.000000 GR
H13a H 0.3606(3) 1.1476(16) 1.4146(3) 0.0425(6) Uiso 1.000000 GR
H13b H 0.4924(16) 1.1074(11) 1.43882(19) 0.0425(6) Uiso 1.000000 GR
H13c H 0.5057(15) 1.2485(5) 1.4180(3) 0.0425(6) Uiso 1.000000 GR
H12a H 1.140(2) 0.7995(15) 1.3502(16) 0.0777(11) Uiso 1.000000 GR
H12b H 1.0186(4) 0.862(2) 1.3474(16) 0.0777(11) Uiso 1.000000 GR
H12c H 1.1557(19) 0.9560(10) 1.4513(3) 0.0777(11) Uiso 1.000000 GR
H11a H 1.1342(7) 0.680(2) 1.5836(16) 0.0677(10) Uiso 1.000000 GR
H11b H 1.1917(15) 0.672(2) 1.4747(3) 0.0677(10) Uiso 1.000000 GR
H11c H 1.2366(9) 0.8262(3) 1.5884(16) 0.0677(10) Uiso 1.000000 GR
H15a H 0.3553(3) 0.0566(3) 0.8032(2) 0.0471(7) Uiso 1.000000 R
H15b H 0.3347(3) 0.0268(3) 0.9117(2) 0.0471(7) Uiso 1.000000 R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Fe 0.35822 0.84933 11.76950 7.35730 3.52220 2.30450 4.76110 0.30720 15.35350
76.88050 1.03690004349
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
O4 Fe1 O1 86.58(5) 2_667 .
O5 Fe1 O1 89.73(5) 2_667 .
O5 Fe1 O4 79.32(5) 2_667 2_667
O7 Fe1 O1 167.75(6) . .
O7 Fe1 O4 84.55(6) . 2_667
O7 Fe1 O5 96.89(6) . 2_667
O2 Fe1 O1 79.16(5) . .
O2 Fe1 O4 84.48(5) . 2_667
O2 Fe1 O5 160.88(5) . 2_667
O2 Fe1 O7 91.58(5) . .
Cl1 Fe1 O1 94.72(4) . .
Cl1 Fe1 O4 177.75(4) . 2_667
Cl1 Fe1 O5 98.84(4) . 2_667
Cl1 Fe1 O7 94.42(5) . .
Cl1 Fe1 O2 97.56(4) . .
C11 S1 O7 102.96(10) . .
C12 S1 O7 103.56(11) . .
C12 S1 C11 101.45(16) . .
C7 O1 Fe1 112.99(11) . .
C9 O4 Fe1 112.43(11) . 2_667
C10 O5 Fe1 118.22(11) . 2_667
S1 O7 Fe1 123.50(8) . .
C8 O2 Fe1 117.18(11) . .
C7 N1 C1 123.24(15) . .
C9 N2 C2 124.89(15) . .
C1 C2 N2 119.48(15) . .
C3 C2 N2 120.91(16) . .
C3 C2 C1 119.58(16) . .
N2 C9 O4 125.64(16) . .
C10 C9 O4 117.91(15) . .
C10 C9 N2 116.44(15) . .
C2 C1 N1 119.48(15) . .
C6 C1 N1 120.26(16) . .
C6 C1 C2 120.26(17) . .
N1 C7 O1 125.27(16) . .
C8 C7 O1 118.18(15) . .
C8 C7 N1 116.55(15) . .
O2 C8 O3 128.09(17) . .
C7 C8 O3 119.53(16) . .
C7 C8 O2 112.37(15) . .
O6 C10 O5 128.11(17) . .
C9 C10 O5 112.08(15) . .
C9 C10 O6 119.80(16) . .
C13 S2 O8 104.70(9) . .
C14 S2 O8 105.58(9) . .
C14 S2 C13 97.98(11) . .
C3 C4 C5 120.28(18) . .
C5 C6 C1 119.85(18) . .
C6 C5 C4 120.01(18) . .
C4 C3 C2 119.98(18) . .
Cl3 C15 Cl2 111.51(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.0801(13) .
Fe1 O4 2.1052(13) 2_667
Fe1 O5 1.9829(13) 2_667
Fe1 O7 1.9764(14) .
Fe1 O2 2.0252(13) .
Fe1 Cl1 2.2489(5) .
S1 O7 1.5356(14) .
S1 C11 1.762(2) .
S1 C12 1.768(3) .
O1 C7 1.249(2) .
O4 C9 1.246(2) .
O5 C10 1.290(2) .
O3 C8 1.222(2) .
O6 C10 1.214(2) .
O2 C8 1.276(2) .
N1 C1 1.430(2) .
N1 C7 1.318(2) .
N2 C2 1.423(2) .
N2 C9 1.317(2) .
C2 C1 1.394(2) .
C2 C3 1.390(2) .
C9 C10 1.541(2) .
C1 C6 1.384(2) .
C7 C8 1.539(2) .
S2 O8 1.5209(14) .
S2 C13 1.778(2) .
S2 C14 1.779(2) .
C4 C5 1.386(3) .
C4 C3 1.384(3) .
C6 C5 1.388(3) .
Cl2 C15 1.752(3) .
Cl3 C15 1.771(3) .
