Two cyclohexane-type octadecanuclear metalla-macrocycle-based metal organic frameworks and adsorption properties
Chen, Shufang; Hu, Jiyong; Zhao, Jin'an; Zhang, Jin; Yu, Huaibin; Zhi, Shuangcheng; Zhang, Junshuai; Gong, Zhanqiang; CrystEngComm 18 (2016) 5353–; doi:10.1039/C6CE00494F

data_7225348
_publ_section_title
;
 Two cyclohexane-type octadecanuclear metalla-macrocycle-based metal
 organic frameworks and adsorption properties
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5353
_journal_paper_doi               10.1039/C6CE00494F
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.02(C2208 H2016 N192 O384 S96 Zn48), H2 O'
_chemical_formula_sum            'C46 H44 N4 O9 S2 Zn'
_chemical_formula_weight         926.34
_space_group_crystal_system      cubic
_space_group_IT_number           230
_space_group_name_Hall           '-I 4bd 2c 3'
_space_group_name_H-M_alt        'I a -3 d'
_symmetry_space_group_name_Hall  '-I 4bd 2c 3'
_symmetry_space_group_name_H-M   'I a -3 d'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-26
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_audit_update_record
;
2016-02-01 deposited with the CCDC.
2016-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            48
_cell_length_a                   42.5590(2)
_cell_length_b                   42.5590(2)
_cell_length_c                   42.5590(2)
_cell_measurement_reflns_used    12318
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6227
_cell_measurement_theta_min      3.2811
_cell_volume                     77085.8(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.5281
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega  -96.00  -48.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4835  125.0000  120.0000 48

  2 omega   48.00   89.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4530  -45.0000  120.0000 41

  3 omega   31.00   69.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4530  -30.0000   90.0000 38

  4 omega -119.00  -85.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4835  -77.0000 -180.0000 34
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0171492000
_diffrn_orient_matrix_UB_12      -0.0100832000
_diffrn_orient_matrix_UB_13      0.0302302000
_diffrn_orient_matrix_UB_21      -0.0314390000
_diffrn_orient_matrix_UB_22      -0.0112321000
_diffrn_orient_matrix_UB_23      0.0140862000
_diffrn_orient_matrix_UB_31      0.0054228000
_diffrn_orient_matrix_UB_32      -0.0328653000
_diffrn_orient_matrix_UB_33      -0.0140949000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            31674
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.777
_diffrn_reflns_theta_min         3.886
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.958
_exptl_crystal_description       block
_exptl_crystal_F_000             23136
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1176P)^2^+158.9407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2056
_refine_ls_wR_factor_ref         0.2479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4252
_reflns_number_total             6325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00494f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7225347--7225348.cif.'
_cod_original_cell_volume        77085.8(11)
_cod_database_code               7225348
_reflns_odcompleteness_completeness 99.73
_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 C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5A
 0.85 with sigma of 0.01
 C4-C5 = C6-C7 = C4'-C5' = C6'-C7'
 1.34 with sigma of 0.01
 C5-C6 = C5'-C6'
 1.5 with sigma of 0.01
 C4-S1 = C7-S1 = C4'-S1' = C7'-S1'
 1.72 with sigma of 0.01
 C20-C21 = C21-C22 = C22-C23 = C20-C21' = C21'-C22' = C22'-C23'
 1.54 with sigma of 0.01
 C20-C22 = C21-C23 = C20-C22' = C21'-C23'
 2.52 with sigma of 0.01
 C5-S1 \\sim C6-S1 \\sim C5'-S1' \\sim C6'-S1'
 with sigma of 0.01
 C4-C6 \\sim C5-C7 \\sim C4'-C6' \\sim C7'-C5'
 with sigma of 0.01
 C3-C4 \\sim C3-C4'
 with sigma of 0.01
3. Restrained planarity
 C3, C4, C5, C6, C7, S1
 with sigma of 0.01
 C3, C4', C5', C6', C7', S1'
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) = Uanis(C7')
Uanis(C7) = Uanis(C6')
Uanis(C21) = Uanis(C21')
Uanis(C23) = Uanis(C23')
Uanis(C22) = Uanis(C22')
Uanis(C5) = Uanis(S1')
Uanis(S1) = Uanis(C5')
Uanis(C4) = Uanis(C4')
5. Others
 Sof(H3C)=Sof(H3D)=Sof(C4')=Sof(C5')=Sof(H5')=Sof(C6')=Sof(H6')=Sof(C7')=
 Sof(H7')=Sof(S1')=1-FVAR(1)
 Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=
 Sof(S1)=FVAR(1)
 Sof(H20C)=Sof(H20D)=Sof(C21')=Sof(H21C)=Sof(H21D)=Sof(C22')=Sof(H22C)=
 Sof(H22D)=Sof(C23')=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(2)
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
6.a Riding coordinates:
 C3(H3A,H3B,H3C,H3D), C20(H20A,H20B,H20C,H20D)
6.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C21'(H21C,H21D), C22'(H22C,H22D)
6.c Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C23'(H23D,H23E,H23F)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C5'(H5'), C6'(H6'), C7'(H7'), C8(H8), C10(H10),
 C14(H14), C15(H15), C17(H17), C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_fab_checksum              41253
_shelx_shelxl_version_number     2014/7