An FeIII dinuclear metallacycle complex as a size-selective adsorbent for nitrogenous compounds and a potentially effective ammonia storage material
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.; Journal of Materials Chemistry A 7 (2019) 15225–; doi:10.1039/C8TA09786K

data_7237241
_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
;
  1 omega  -76.00   12.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082  -38.0000  -90.0000 88

  2 omega  -41.00   59.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082   38.0000   90.0000 100

  3 omega  -17.00   85.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957   77.0000 -180.0000 102

  4 omega   58.00  107.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957  179.0000    0.0000 49

  5 omega   64.00   90.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957 -153.0000   72.0000 26

  6 omega -104.00  -32.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082  179.0000  150.0000 72

  7 omega  -93.00   19.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082  -77.0000 -180.0000 112

  8 omega  -91.00   12.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -      -14.6082  -38.0000   30.0000 103

  9 omega  -59.00   28.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957  -38.0000  -30.0000 87

 10 omega   16.00   41.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957 -122.0000 -134.0000 25

 11 omega   16.00   72.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957 -122.0000   52.0000 56

 12 omega  -59.00   28.00   1.0000   20.3400
omega____ theta____ kappa____ phi______ frames
    -       16.7957  -38.0000  150.0000 87

 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       '\w 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/[\s^2^(Fo^2^)+(0.0393P)^2^+1.3391P] where P=(Fo^2^+2Fc^2^)/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'