Interplaying anions in a supramolecular metallohydrogel to form metal organic frameworks.
Karak, Suvendu; Kumar, Sushil; Bera, Saibal; Díaz, David Díaz; Banerjee, Subhrashis; Vanka, Kumar; Banerjee, Rahul; Chemical communications (Cambridge, England) 53 (2017) 3705–3708; doi:10.1039/c7cc00539c

data_7119741
_publ_section_title
;
 Interplaying anions in a supramolecular metallohydrogel to form metal
 organic frameworks.
;
_journal_issue                   26
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3705
_journal_page_last               3708
_journal_paper_doi               10.1039/c7cc00539c
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C24 H24 N6 O6, 4(C2 H6 O S)'
_chemical_formula_sum            'C32 H48 N6 O10 S4'
_chemical_formula_weight         805.00
_chemical_name_common            TpEDA
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1my6pg
_audit_creation_date             2016-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2016-11-16 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.934(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.165(3)
_cell_length_b                   10.8543(10)
_cell_length_c                   20.384(3)
_cell_measurement_reflns_used    1719
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.9090
_cell_measurement_theta_min      3.8300
_cell_volume                     3778.3(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1640
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.846
_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    -48.00  44.00   1.00   61.30    --   20.06 -77.00 -90.00   92
  2  \w    -12.00  64.00   1.00   61.30    --   20.06 -99.00  60.00   76
  3  \w     56.00  82.00   1.00   61.30    --   20.06-178.00  90.00   26
  4  \w    -87.00 -49.00   1.00   61.30    --  -20.37 -37.00 120.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0265822000
_diffrn_orient_matrix_UB_12      -0.0397868000
_diffrn_orient_matrix_UB_13      0.0080789000
_diffrn_orient_matrix_UB_21      0.0308175000
_diffrn_orient_matrix_UB_22      -0.0421371000
_diffrn_orient_matrix_UB_23      0.0156836000
_diffrn_orient_matrix_UB_31      0.0080572000
_diffrn_orient_matrix_UB_32      0.0301103000
_diffrn_orient_matrix_UB_33      0.0326999000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7609
_diffrn_reflns_theta_full        29.24
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         3.35
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         5143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.1026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1791P)^2^+4.5972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2777
_refine_ls_wR_factor_ref         0.3271
_reflns_number_gt                4613
_reflns_number_total             5143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc00539c2.cif
_cod_data_source_block           TpEDA
_cod_depositor_comments
'Adding full bibliography for 7119741--7119744.cif.'
_cod_database_code               7119741
_chemical_oxdiff_formula         'C10 H10 N10 O10'
_reflns_odcompleteness_completeness 99.56
_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 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:
 C16(H16a,H16b), C17(H17a,H17b), C18(H18a,H18b)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), C7(H7), C10(H10), C13(H13)
2.c Idealised Me refined as rotating group:
 C20(H20a,H20b,H20c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,
 H24c)
;
_olex2_date_sample_data_collection 1476527428.97
_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 4.618
_oxdiff_exptl_absorpt_empirical_full_min 0.512