Rational Construction of Breathing Metal-Organic Frameworks through Synergy of a Stretchy Ligand and Highly Variable π-π Interaction.
Zhang, Ying; Meng, Xiao-Qing; Ding, Hao-Jing; Wang, Xi; Yu, Mei-Hui; Zhang, Shu-Ming; Chang, Ze; Bu, Xian-He; ACS applied materials & interfaces 11 (2019) 20995–21003; doi:10.1021/acsami.9b04759

data_4514575
_publ_section_title
;
 Rational Construction of Breathing Metal-Organic Frameworks through
 Synergy of a Stretchy Ligand and Highly Variable \p-\p Interaction.
;
_journal_issue                   23
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              20995
_journal_page_last               21003
_journal_paper_doi               10.1021/acsami.9b04759
_journal_volume                  11
_journal_year                    2019
_chemical_formula_moiety         'C64 H40 Cd2 N16 O8'
_chemical_formula_sum            'C64 H40 Cd2 N16 O8'
_chemical_formula_weight         1385.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                77.504(3)
_cell_angle_beta                 66.142(4)
_cell_angle_gamma                88.035(3)
_cell_formula_units_Z            2
_cell_length_a                   15.0446(6)
_cell_length_b                   15.3208(6)
_cell_length_c                   18.3342(6)
_cell_measurement_reflns_used    19402
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      74.4910
_cell_measurement_theta_min      4.1360
_cell_volume                     3766.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -88.00  35.00   0.50    0.50    --    0.00 -82.00-120.00  246
  2  \w    -23.00   5.00   0.50    0.50    --    0.00  77.00 -90.00   56
  3  \w    -64.00 -36.00   0.50    0.50    --    0.00 -77.00  30.00   56
  4  \w      2.00  83.00   0.50    0.50    --    0.00  57.00 -60.00  162
  5  \w    -67.00 -31.00   0.50    0.50    --    0.00 -38.00  60.00   72
  6  \w     -8.00  18.00   0.50    0.50    --    0.00 -38.00  60.00   52
  7  \w    -29.00  82.00   0.50    0.50    --    0.00  57.00  90.00  222
  8  \w     63.00 182.00   0.50    0.50    --   97.10  30.00   0.00  238
  9  \w     63.00 186.00   0.50    0.50    --   97.10  30.00 -30.00  246
 10  \w      9.00 134.00   0.50    0.50    --   97.10 -82.00 -90.00  250
 11  \w     75.00 102.00   0.50    0.50    --   97.10 -82.00-150.00   54
 12  \w     70.00 133.00   0.50    0.50    --   97.10 -82.00   0.00  126
 13  \w      9.00  72.00   0.50    0.50    --   97.10 -82.00  90.00  126
 14  \w     94.00 119.00   0.50    0.50    --   97.10 -82.00-180.00   50
 15  \w     55.00 129.00   0.50    0.50    --   97.10 -82.00 120.00  148
 16  \w     68.00 180.00   0.50    0.50    --   97.10  61.00-120.00  224
 17  \w      9.00 131.00   0.50    0.50    --   97.10 -30.00   0.00  244
 18  \w    115.00 142.00   0.50    0.50    --   97.10  61.00  60.00   54
 19  \w     10.00 128.00   0.50    0.50    --   97.10 -61.00 120.00  236
 20  \w     17.00 123.00   0.50    0.50    --   97.10 -61.00 -90.00  212
 21  \w    112.00 150.00   0.50    0.50    --   97.10  44.00  30.00   76
 22  \w     65.00 106.00   0.50    0.50    --   97.10 -82.00  60.00   82
 23  \w     93.00 120.00   0.50    0.50    --   97.10 -82.00-120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0058032000
_diffrn_orient_matrix_UB_12      0.0993095000
_diffrn_orient_matrix_UB_13      -0.0368883000
_diffrn_orient_matrix_UB_21      -0.1119271000
_diffrn_orient_matrix_UB_22      -0.0123138000
_diffrn_orient_matrix_UB_23      0.0372135000
_diffrn_orient_matrix_UB_31      -0.0044609000
_diffrn_orient_matrix_UB_32      0.0251301000
_diffrn_orient_matrix_UB_33      0.0783049000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41275
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.993
_diffrn_reflns_theta_min         3.539
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.990
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.338
_refine_diff_density_min         -2.867
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         14853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0568
_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^)+(0.1032P)^2^+2.3289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13198
_reflns_number_total             14853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b04759_si_007.cif
_cod_data_source_block           1'c
_cod_database_code               4514575
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.502
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25), C26(H26),
  C28(H28), C29(H29), C31(H31), C32(H32), C36(H36), C37(H37), C39(H39),
 C40(H40), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51),
  C52(H52), C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C64(H64),
 C65(H65), C66(H66)
;
_shelx_res_checksum              55070
_shelx_hkl_checksum              54883
_shelx_fab_checksum              12912
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.812
_oxdiff_exptl_absorpt_empirical_full_min 0.577