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_4514576
_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         'C128 H80 Cd4 N32 O16'
_chemical_formula_sum            'C128 H80 Cd4 N32 O16'
_chemical_formula_weight         2771.84
_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                82.8120(10)
_cell_angle_beta                 82.5980(10)
_cell_angle_gamma                68.3390(10)
_cell_formula_units_Z            2
_cell_length_a                   18.4591(2)
_cell_length_b                   20.0087(3)
_cell_length_c                   21.7899(3)
_cell_measurement_reflns_used    39661
_cell_measurement_temperature    298.00(10)
_cell_measurement_theta_max      73.9940
_cell_measurement_theta_min      3.7420
_cell_volume                     7390.98(18)
_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      air
_diffrn_ambient_temperature      298.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.964
_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    -84.00  -1.00   0.50    0.50    --    0.00 -62.00  55.00  166
  2  \w    -88.00  30.00   0.50    0.50    --    0.00 -57.00 120.00  236
  3  \w    -89.00 -21.00   0.50    0.50    --    0.00 -38.00 -90.00  136
  4  \w    -88.00 -25.00   0.50    0.50    --    0.00 -57.00-150.00  126
  5  \w     78.00 131.00   0.50    0.68    --   95.80 -30.00 150.00  106
  6  \w      7.00 119.00   0.50    0.68    --   95.80 -45.00  60.00  224
  7  \w     80.00 107.00   0.50    0.68    --   95.80 -82.00 120.00   54
  8  \w     60.00 184.00   0.50    0.68    --   95.80  30.00  60.00  248
  9  \w     14.00  39.00   0.50    0.68    --   95.80 -30.00 150.00   50
 10  \w     11.00 106.00   0.50    0.68    --   95.80 -82.00-150.00  190
 11  \w     53.00 132.00   0.50    0.68    --   95.80 -82.00  30.00  158
 12  \w     71.00 105.00   0.50    0.68    --   95.80 -82.00  90.00   68
 13  \w     64.00  93.00   0.50    0.68    --   95.80  30.00 120.00   58
 14  \w    108.00 184.00   0.50    0.68    --   95.80  30.00 120.00  152
 15  \w      7.00  32.00   0.50    0.68    --   95.80 -82.00  60.00   50
 16  \w     97.00 148.00   0.50    0.68    --   95.80  77.00  90.00  102
 17  \w     80.00 132.00   0.50    0.68    --   95.80 -82.00 -60.00  104
 18  \w     94.00 129.00   0.50    0.68    --   95.80 -82.00  60.00   70
 19  \w     14.00  47.00   0.50    0.68    --   95.80 -82.00-180.00   66
 20  \w     78.00 103.00   0.50    0.68    --   95.80 -82.00-180.00   50
 21  \w      6.00 123.00   0.50    0.68    --   95.80 -61.00-150.00  234
 22  \w     46.00  72.00   0.50    0.68    --   95.80 -82.00 -30.00   52
 23  \w     97.00 123.00   0.50    0.68    --   95.80 -82.00 -30.00   52
 24  \w     29.00  55.00   0.50    0.68    --   95.80 -82.00  90.00   52
 25  \w     14.00 115.00   0.50    0.68    --   95.80 -45.00 -60.00  202
 26  \w     50.00 132.00   0.50    0.68    --   95.80 -82.00-120.00  164
 27  \w     18.00  70.00   0.50    0.68    --   95.80 -82.00 120.00  104
;
_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      -0.0236116000
_diffrn_orient_matrix_UB_12      0.0720559000
_diffrn_orient_matrix_UB_13      0.0293708000
_diffrn_orient_matrix_UB_21      -0.0670401000
_diffrn_orient_matrix_UB_22      0.0341792000
_diffrn_orient_matrix_UB_23      -0.0426056000
_diffrn_orient_matrix_UB_31      -0.0554741000
_diffrn_orient_matrix_UB_32      -0.0234935000
_diffrn_orient_matrix_UB_33      0.0494099000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            89982
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.573
_diffrn_reflns_theta_min         3.734
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60986
_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    1.246
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.009
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1621
_refine_ls_number_reflns         29165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+2.3371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23326
_reflns_number_total             29165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b04759_si_006.cif
_cod_data_source_block           1c
_cod_database_code               4514576
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.630
_shelx_estimated_absorpt_t_min   0.497
_reflns_odcompleteness_completeness 99.51
_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:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27),
  C31(H31), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39), C40(H40),
 C42(H42), C46(H46), C47(H47), C49(H49), C50(H50), C52(H52), C53(H53), C55(H55),
  C56(H56), C58(H58), C59(H59), C61(H61), C62(H62), C67(H67), C68(H68),
 C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C80(H80), C85(H85), C86(H86), C87(H87), C88(H88), C90(H90),
 C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C97(H97), C98(H98),
 C103(H103), C104(H104), C105(H105), C106(H106), C108(H108), C109(H109),
 C110(H110), C111(H111), C112(H112), C113(H113), C114(H114), C115(H115),
 C121(H121), C122(H122), C123(H123), C124(H124), C126(H126), C127(H127),
 C128(H128), C129(H129)
;
_shelx_res_checksum              79418
_shelx_hkl_checksum              14042
_shelx_fab_checksum              49795
_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 1.521
_oxdiff_exptl_absorpt_empirical_full_min 0.653