A cage-based cationic body-centered tetragonal metal-organic framework: single-crystal to single-crystal transformation and selective uptake of organic dyes
Di-ming Chen; Wei Shi; Peng Cheng; Chem.Commun. 51 (2015) 370–; doi:10.1039/C4CC07357F

data_7116357
_publ_section_title
;
 A cage-based cationic body-centered tetragonal metal-organic framework:
 single-crystal to single-crystal transformation and selective uptake of
 organic dyes
;
_journal_name_full               Chem.Commun.
_journal_page_first              370
_journal_paper_doi               10.1039/C4CC07357F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C61 H84 Cl Cu4 N17 O20.50, 3(N O3)'
_chemical_formula_sum            'C61 H84 Cl Cu4 N20 O29.5'
_chemical_formula_weight         1859.09
_chemical_name_systematic        1
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9590(3)
_cell_length_b                   13.9590(3)
_cell_length_c                   20.0475(10)
_cell_measurement_reflns_used    2964
_cell_measurement_temperature    139(2)
_cell_measurement_theta_max      28.2670
_cell_measurement_theta_min      3.4200
_cell_volume                     3906.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      139(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   24.00   59.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000  -30.0000 35

  2 omega   49.00   76.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  178.0000   60.0000 27

  3 omega  -12.00   19.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -57.0000    0.0000 31

  4 omega   12.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   77.0000 -120.0000 59

  5 omega  -54.00   44.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -37.0000   60.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0080000000
_diffrn_orient_matrix_UB_12      -0.0397738000
_diffrn_orient_matrix_UB_13      -0.0212353000
_diffrn_orient_matrix_UB_21      0.0408905500
_diffrn_orient_matrix_UB_22      0.0231892500
_diffrn_orient_matrix_UB_23      -0.0135407500
_diffrn_orient_matrix_UB_31      0.0292159000
_diffrn_orient_matrix_UB_32      -0.0215243000
_diffrn_orient_matrix_UB_33      0.0247601000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8586
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1918
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
The remaining solvent molecules were disordered and assigned as 10 NMP and 7 H2O molecules per unit cell according to the TGA and elemental analysis results. The contributions of these disordered solvent to the scattering values have been removed by using the PLATON SQUEEZE program. The total  unit  cell include 10 NMP and 7 H2O molecules (54e*10+7*10=610e), SQUEEZE result reveals that 328 electrons were removed from the unit cell. This discrepancy might be owing to the moderate quality of low angle data caused by the highly disordered framework. 
;
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1026
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0927P)^2^+20.9483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                947
_reflns_number_total             1026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07357f2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C61 H84 Cl Cu4 N20 O29.50'
_cod_database_code               7116357
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{N1A, C1B}
2. Others
 Fixed Sof: N3(0.5) C1B(0.25) C6(0.25) C7(0.25) C8(0.5) H8(0.5) C10(0.5)
 H10(0.5) O1(0.25) H1A(0.25) H1B(0.25) O6(0.5) N1A(0.25) H3(0.5) O1AA(0.1875)
 O0AA(0.375) N6(0.1875)
 Fixed U12: Cu1(0) Cl2(0) O1AA(0) O0AA(0) N6(0)
 Fixed U13: Cu1(0) Cl2(0) O1(0) O1AA(0) O0AA(0) N6(0)
 Fixed U23: Cu1(0) Cl2(0) O1(0) O1AA(0) N6(0)
 Fixed Uiso: H8(0.028) H10(0.067) H1A(0.105) H1B(0.105) H3(0.031)
 Fixed X: Cu1(0) Cl2(0) H8(-0.0853) H10(-0.1026) H1A(0.0275) H1B(-0.036)
 O1AA(0) O0AA(0) N6(0)
 Fixed Y: Cl2(0) H8(0.285) H10(0.3037) H1A(0.3975) H1B(0.3907) O1AA(0.5) N6(0.5)
 Fixed Z: Cu1(0) Cl2(0) C3(0.25) H8(0.1316) H10(0.173) O1(0) H1A(-0.017)
 H1B(0.0436)
;
_olex2_submission_special_instructions 'No special instructions were received'