The Crystalline Sponge Method: A Solvent-Based Strategy to Facilitate Noncovalent Ordered Trapping of Solid and Liquid Organic Compounds
Ramadhar, Timothy R.; Zheng, Shao-Liang; Chen, Yu-Sheng; Clardy, Jon; CrystEngComm  (2017) –; doi:10.1039/C7CE00885F

data_7228689
_publ_section_title
;
 The Crystalline Sponge Method: A Solvent-Based Strategy to Facilitate
 Noncovalent Ordered Trapping of Solid and Liquid Organic Compounds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00885F
_journal_year                    2017
_chemical_formula_moiety
'C36 H24 I6 N12 Zn3, 0.68(C5 H12 O), 0.66(C7 H4 F3 N3)'
_chemical_formula_sum            'C44.03 H34.79 F1.99 I6 N13.99 O0.68 Zn3'
_chemical_formula_weight         1765.98
_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
_audit_creation_date             2017-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-04-24 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.8270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.2912(17)
_cell_length_b                   14.8832(7)
_cell_length_c                   30.9415(15)
_cell_measurement_reflns_used    9541
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.243
_cell_measurement_theta_min      2.190
_cell_volume                     15906.9(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2014.3 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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    'SHELXTL XT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX II CCD Detector'
_diffrn_detector_type            'Bruker APEX II CCD Detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Si 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            113242
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        14.262
_diffrn_reflns_theta_max         14.262
_diffrn_reflns_theta_min         0.782
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.9356
_exptl_absorpt_correction_T_min  0.8284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1317 before and 0.0730 after correction. The Ratio of minimum to maximum transmission is 0.8854. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       prism
_exptl_crystal_F_000             6626
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.614
_refine_diff_density_min         -2.097
_refine_diff_density_rms         0.430
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         14007
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1337P)^2^+128.1977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2032
_refine_ls_wR_factor_ref         0.2271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11742
_reflns_number_total             14007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00885f2.cif
_cod_data_source_block           zni2mof-cf3phenylazide_a
_cod_database_code               7228689
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.817
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N13, N13A}
{N14, N14A}
{N15, N15A}
{C42, C42A}
{C43, C43A}
{C44, C44A}
{C45, C45A}
{C46, C46A}
{C47, C47A}
{C48, C48A}
3. Restrained distances
 C40-C37 \\sim C40-C38 \\sim C40-C39
 with sigma of 0.02
 C45-C46 \\sim C45-C44
 with sigma of 0.02
 C46-C47 \\sim C43-C44
 with sigma of 0.02
 C42-C47 \\sim C43-C42
 with sigma of 0.02
 C47-N15 \\sim C43-N15
 with sigma of 0.02
 C48-F1 \\sim C48A-F1A \\sim C48-F2 \\sim C48A-F2A \\sim C48-F3 \\sim C48A-F3A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Zn1) = Uanis(Zn1A)
Uanis(I1) = Uanis(I1A)
Uanis(I2) = Uanis(I2A)
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(F3) = Uanis(F3A)
Uanis(N13) = Uanis(N13A)
Uanis(N14) = Uanis(N14A)
Uanis(N15) = Uanis(N15A)
Uanis(C42) = Uanis(C42A)
Uanis(C43) = Uanis(C43A)
Uanis(C44) = Uanis(C44A)
Uanis(C45) = Uanis(C45A)
Uanis(C46) = Uanis(C46A)
Uanis(C47) = Uanis(C47A)
Uanis(C48) = Uanis(C48A)
5. Rigid body (RIGU) restrains
 C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44, C45, C46, C48, F1, F2, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Zn1A)=Sof(I1A)=Sof(I2A)=1-FVAR(1)
 Sof(Zn1)=Sof(I1)=Sof(I2)=FVAR(1)
 Sof(O1)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=FVAR(2)
 Sof(N13)=Sof(N14)=Sof(N15)=Sof(C42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=
 Sof(C45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(F1)=Sof(F2)=Sof(F3)=
 FVAR(3)
 Sof(N13A)=Sof(N14A)=Sof(N15A)=Sof(C42A)=Sof(C43A)=Sof(H43A)=Sof(C44A)=
 Sof(H44A)=Sof(C45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(F1A)=
 Sof(F2A)=Sof(F3A)=FVAR(4)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C43(H43), C44(H44), C46(H46), C47(H47), C43A(H43A), C44A(H44A), C46A(H46A),
 C47A(H47A)
7.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C)
;
_shelx_res_checksum              16844
_olex2_submission_special_instructions 'No special instructions were received'