Infinite coordination polymer networks: metallogelation of aminopyridine conjugates and in situ silver nanoparticle formation.
Tatikonda, Rajendhraprasad; Bulatov, Evgeny; Özdemir, Zülal; Nonappa, ?; Haukka, Matti; Soft matter 15 (2019) 442–451; doi:10.1039/c8sm02006j

data_1550351
_publ_section_title
;
 Infinite coordination polymer networks: metallogelation of aminopyridine
 conjugates and in situ silver nanoparticle formation.
;
_journal_issue                   3
_journal_name_full               'Soft matter'
_journal_page_first              442
_journal_page_last               451
_journal_paper_doi               10.1039/c8sm02006j
_journal_volume                  15
_journal_year                    2019
_chemical_formula_moiety         '2(C2 H6 O S), C22 H16 N6 O2'
_chemical_formula_sum            'C26 H28 N6 O4 S2'
_chemical_formula_weight         552.66
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-03-15 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                89.276(6)
_cell_angle_beta                 72.988(6)
_cell_angle_gamma                79.287(6)
_cell_formula_units_Z            1
_cell_length_a                   7.4404(5)
_cell_length_b                   9.0236(7)
_cell_length_c                   10.0764(7)
_cell_measurement_reflns_used    4656
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.8450
_cell_measurement_theta_min      3.3430
_cell_volume                     635.02(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -39.00  47.00   1.00    9.00    --  -18.14  57.00 -60.00   86
  2  \w      4.00  30.00   1.00    9.00    --   19.23  57.00  30.00   26
  3  \w     -6.00  86.00   1.00    9.00    --   19.23  77.00  60.00   92
  4  \w    -10.00  85.00   1.00    9.00    --   19.23  77.00 -90.00   95
  5  \w      5.00  79.00   1.00    9.00    --   19.23  57.00-180.00   74
  6  \w    -39.00  51.00   1.00    9.00    --  -18.14  57.00  30.00   90
  7  \w    -45.00  63.00   1.00    9.00    --   19.23 -19.00 120.00  108
  8  \w    -20.00  61.00   1.00    9.00    --   19.23 -99.00 120.00   81
  9  \w     40.00  79.00   1.00    9.00    --   19.23-128.00 -53.72   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0083687000
_diffrn_orient_matrix_UB_12      0.0789853000
_diffrn_orient_matrix_UB_13      0.0096941000
_diffrn_orient_matrix_UB_21      -0.0833101000
_diffrn_orient_matrix_UB_22      0.0016407000
_diffrn_orient_matrix_UB_23      0.0570377000
_diffrn_orient_matrix_UB_31      0.0574689000
_diffrn_orient_matrix_UB_32      -0.0130838000
_diffrn_orient_matrix_UB_33      0.0456332000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8538
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.055
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             290
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0318
_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/[\s^2^(Fo^2^)+(0.0282P)^2^+0.3593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2316
_reflns_number_total             2591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sm02006j2.cif
_cod_data_source_block           4inDMSO
_cod_depositor_comments
'Adding full bibliography for 1550349--1550355.cif.'
_cod_original_cell_volume        635.01(8)
_cod_database_code               1550351
_chemical_oxdiff_formula         'C24 H16 N6 O3 S'
_chemical_oxdiff_usercomment     'Clear, colrless, block, 0.2 0.18 0.08'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C5(H5), C10(H10), C3(H3), C7(H7), C2(H2A), C9(H9), C8(H8)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C)
;
_shelx_shelxl_version_number     2014/7
_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 1.387
_oxdiff_exptl_absorpt_empirical_full_min 0.825