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_7228687
_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, 2.04(C14 H12)'
_chemical_formula_sum            'C64.56 H48.48 I6 N12 Zn3'
_chemical_formula_weight         1949.83
_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             2017-04-20
_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                 107.5655(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.9049(14)
_cell_length_b                   14.9409(6)
_cell_length_c                   34.5319(14)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    100
_cell_measurement_theta_max      14.206
_cell_measurement_theta_min      2.258
_cell_volume                     17169.1(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_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
_diffrn_detector                 'Pilatus 1M CdTe Pixel Array Detector'
_diffrn_detector_type            'Pilatus 1M CdTe Pixel Array Detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device
'Huber three-circle goniometer with free kappa'
_diffrn_measurement_device_type
'Huber three-circle goniometer with free kappa'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Si 1 1 1'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            176286
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         14.380
_diffrn_reflns_theta_min         0.980
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.9515
_exptl_absorpt_correction_T_min  0.8844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0716 before and 0.0555 after correction. The Ratio of minimum to maximum transmission is 0.9295. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       prism
_exptl_crystal_F_000             7423
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.965
_refine_diff_density_min         -1.692
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         15424
_refine_ls_number_restraints     573
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1106P)^2^+110.0348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.1811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13344
_reflns_number_total             15424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00885f2.cif
_cod_data_source_block           tim73-transstilbene-mtbe_a
_cod_original_cell_volume        17169.0(12)
_cod_database_code               7228687
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Zn1-N7 \\sim Zn1A-N7
 with sigma of 0.02
 Zn3-N9 \\sim Zn3A-N9
 with sigma of 0.02
 C51-C56 \\sim C55-C56
 with sigma of 0.02
 C51-C52 \\sim C55-C54
 with sigma of 0.02
 C52-C53 \\sim C54-C53
 with sigma of 0.02
 C59-C60 \\sim C59-C64
 with sigma of 0.02
 C60-C61 \\sim C64-C63
 with sigma of 0.02
 C61-C62 \\sim C63-C62
 with sigma of 0.02
 C57-C56 \\sim C58-C59
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C70 \\sim C65 \\sim C66: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C71 \\sim C72: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C74 \\sim C75 \\sim C76: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(Zn1) = Uanis(Zn1A)
Uanis(I1) = Uanis(I1A)
Uanis(I2) = Uanis(I2A)
Uanis(Zn3) = Uanis(Zn3A)
Uanis(I5) = Uanis(I5A)
Uanis(I6) = Uanis(I6A)
Uanis(C44) = Uanis(C43A)
Uanis(C45) = Uanis(C42A)
Uanis(C46) = Uanis(C41A)
Uanis(C47) = Uanis(C40A)
Uanis(C48) = Uanis(C39A)
Uanis(C49) = Uanis(C38A)
Uanis(C50) = Uanis(C37A)
Uanis(C37) = Uanis(C50)
Uanis(C38) = Uanis(C49)
Uanis(C39) = Uanis(C48)
Uanis(C40) = Uanis(C47)
Uanis(C41) = Uanis(C46)
Uanis(C42) = Uanis(C45)
Uanis(C43) = Uanis(C44)
Uanis(C37A) = Uanis(C50A)
Uanis(C38A) = Uanis(C49A)
Uanis(C39A) = Uanis(C48A)
Uanis(C40A) = Uanis(C47A)
Uanis(C41A) = Uanis(C46A)
Uanis(C42A) = Uanis(C45A)
Uanis(C43A) = Uanis(C44A)
Uanis(C65) = Uanis(C65A)
Uanis(C66) = Uanis(C66A)
Uanis(C67) = Uanis(C67A)
Uanis(C68) = Uanis(C68A)
Uanis(C69) = Uanis(C69A)
Uanis(C70) = Uanis(C70A)
Uanis(C65A) = Uanis(C78A)
Uanis(C66A) = Uanis(C77A)
Uanis(C67A) = Uanis(C76A)
Uanis(C68A) = Uanis(C75A)
Uanis(C69A) = Uanis(C74A)
Uanis(C70A) = Uanis(C73A)
Uanis(C71A) = Uanis(C72A)
4. Rigid body (RIGU) restrains
 C42, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49, C50} sigma
for 1-2: 0.01, 1-3: 0.02
{C37A, C38A, C39A, C40A, C41A, C42A, C43A, C44A, C45A, C46A, C47A, C48A, C49A,
C50A} sigma for 1-2: 0.01, 1-3: 0.02
{C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78} sigma
for 1-2: 0.01, 1-3: 0.02
{C65A, C66A, C67A, C68A, C69A, C70A, C71A, C72A, C73A, C74A, C75A, C76A, C77A,
C78A} sigma for 1-2: 0.01, 1-3: 0.02
as
{C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64}
6. Others
 Sof(Zn3A)=Sof(I5A)=Sof(I6A)=1-FVAR(1)
 Sof(Zn3)=Sof(I5)=Sof(I6)=FVAR(1)
 Sof(Zn1A)=Sof(I1A)=Sof(I2A)=1-FVAR(2)
 Sof(Zn1)=Sof(I1)=Sof(I2)=FVAR(2)
 Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=
 Sof(C41)=Sof(H41)=Sof(C42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=
 Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=
 Sof(C50)=Sof(H50)=FVAR(3)
 Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=
 Sof(C55)=Sof(H55)=Sof(C56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=Sof(C59)=
 Sof(C60)=Sof(H60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=
 Sof(C64)=Sof(H64)=FVAR(4)
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=
 Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(C43A)=Sof(H43A)=Sof(C44A)=
 Sof(H44A)=Sof(C45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(C48A)=
 Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(H50A)=FVAR(5)
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67)=Sof(C68)=Sof(H68)=
 Sof(C69)=Sof(H69)=Sof(C70)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72)=Sof(C73)=
 Sof(C74)=Sof(H74)=Sof(C75)=Sof(H75)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77)=
 Sof(C78)=Sof(H78)=FVAR(6)
 Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=Sof(C67A)=Sof(H67A)=Sof(C68A)=
 Sof(H68A)=Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(C71A)=Sof(H71A)=Sof(C72A)=
 Sof(H72A)=Sof(C73A)=Sof(C74A)=Sof(H74A)=Sof(C75A)=Sof(H75A)=Sof(C76A)=
 Sof(H76A)=Sof(C77A)=Sof(H77A)=Sof(C78A)=Sof(H78A)=FVAR(7)
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),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C37A(H37A), C38A(H38A), C39A(H39A),
 C40A(H40A), C41A(H41A), C43A(H43A), C44A(H44A), C46A(H46A), C47A(H47A),
 C48A(H48A), C49A(H49A), C50A(H50A), C51(H51), C52(H52), C53(H53), C54(H54),
 C55(H55), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64),
  C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C71(H71), C72(H72),
 C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C65A(H65A), C66A(H66A),
 C67A(H67A), C68A(H68A), C69A(H69A), C71A(H71A), C72A(H72A), C74A(H74A),
 C75A(H75A), C76A(H76A), C77A(H77A), C78A(H78A)
;
_shelx_res_checksum              6628
_olex2_submission_special_instructions 'No special instructions were received'