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_7119744
_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         'C27 H28 N6 O6, O2, 2(H O), 6(H2 O)'
_chemical_formula_sum            'C27 H42 N6 O16'
_chemical_formula_weight         706.67
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2a 2a'
_space_group_name_H-M_alt        'I m m b'
_symmetry_space_group_name_Hall  '-I 2a 2a'
_symmetry_space_group_name_H-M   'I m m b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1my6qh
_audit_creation_date             2016-11-11
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.752(4)
_cell_length_b                   12.9206(16)
_cell_length_c                   11.2524(13)
_cell_measurement_reflns_used    1267
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      63.2280
_cell_measurement_theta_min      4.3850
_cell_volume                     3307.9(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega   22.00   68.00   1.0000    1.8800
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 46

  2 omega   24.00   57.00   1.0000    1.8800
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   90.0000 33

  3 omega   97.00  123.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   30.0000 26

  4 omega   79.00  105.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000   30.0000 26

  5 omega   60.00   89.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  -30.0000 29

  6 omega   43.00   81.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000  -30.0000 38

  7 omega   54.00   88.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000 -180.0000 34

  8 omega   79.00  123.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 44

  9 omega  127.00  174.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 47

 10 omega   39.00   94.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -60.0000 55

 11 omega   34.00   75.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 41

 12 omega   33.00   91.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   30.0000 58

 13 omega   41.00  129.00   1.0000    7.5200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000  120.0000 88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0552780000
_diffrn_orient_matrix_UB_12      -0.0283271000
_diffrn_orient_matrix_UB_13      -0.0723563000
_diffrn_orient_matrix_UB_21      -0.0230003000
_diffrn_orient_matrix_UB_22      -0.1115760000
_diffrn_orient_matrix_UB_23      -0.0137425000
_diffrn_orient_matrix_UB_31      -0.0317782000
_diffrn_orient_matrix_UB_32      0.0307724000
_diffrn_orient_matrix_UB_33      -0.1153442000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3760
_diffrn_reflns_theta_full        70.95
_diffrn_reflns_theta_max         70.95
_diffrn_reflns_theta_min         4.38
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           n/a
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.003(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.666
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1720
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      3.271
_refine_ls_R_factor_all          0.1641
_refine_ls_R_factor_gt           0.1359
_refine_ls_shift/su_max          0.0022
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4260
_refine_ls_wR_factor_ref         0.4806
_reflns_number_gt                907
_reflns_number_total             1679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc00539c2.cif
_cod_data_source_block           TpPDA
_cod_depositor_comments
'Adding full bibliography for 7119741--7119744.cif.'
_cod_database_code               7119744
_chemical_oxdiff_formula         'C12 H14 N4 O6'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O2-H2 = O2-H2_$1
 0.85 with sigma of 0.01
 O4-H4 = O4-H4_$2
 0.85 with sigma of 0.01
 H2_$1-H2
 1.387434 with sigma of 0.02
 H4_$2-H4
 1.387434 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: H8a(0.25) H8b(0.25) C14(0.5) H14(0.5)
5.a Free rotating group:
 O3(H3a,H3b)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16a,H16b), C18(H18a,H18b), C8(H8a,H8b)
5.c Aromatic/amide H refined with riding coordinates:
 N8(H8), C11(H11)
;
_olex2_date_sample_data_collection 1446634335.16
_olex2_submission_special_instructions 'No special instructions were received'