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_4514578
_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                101.054(2)
_cell_angle_beta                 111.350(2)
_cell_angle_gamma                90.981(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8086(4)
_cell_length_b                   15.9794(5)
_cell_length_c                   18.2659(3)
_cell_measurement_reflns_used    22793
_cell_measurement_temperature    298.33(10)
_cell_measurement_theta_max      72.9950
_cell_measurement_theta_min      4.2080
_cell_volume                     3933.09(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.33(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_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     50.00  88.00   0.50    0.50    --    0.00  57.00  90.00   76
  2  \w     -4.00  23.00   0.50    0.50    --    0.00 -82.00-120.00   54
  3  \w     57.00  84.00   0.50    0.50    --    0.00  57.00-150.00   54
  4  \w    -88.00 -11.00   0.50    0.50    --    0.00 -82.00-120.00  154
  5  \w    -28.00  34.00   0.50    0.50    --    0.00  57.00  90.00  124
  6  \w     14.00  89.00   0.50    0.50    --    0.00  57.00 -60.00  150
  7  \w    -30.00  19.00   0.50    0.50    --    0.00  38.00 -60.00   98
  8  \w    -21.00   4.00   0.50    0.50    --    0.00  57.00-150.00   50
  9  \w     49.00 108.00   0.50    0.50    --   98.20 -61.00-120.00  118
 10  \w     69.00 123.00   0.50    0.50    --   98.20 -82.00-120.00  108
 11  \w     11.00  37.00   0.50    0.50    --   98.20 -61.00-120.00   52
 12  \w     23.00 113.00   0.50    0.50    --   98.20 -30.00 -90.00  180
 13  \w     18.00 137.00   0.50    0.50    --   98.20 -82.00 150.00  238
 14  \w     10.00  36.00   0.50    0.50    --   98.20 -82.00-120.00   52
 15  \w     89.00 114.00   0.50    0.50    --   98.20 -82.00  60.00   50
 16  \w     74.00 121.00   0.50    0.50    --   98.20 -45.00 -30.00   94
 17  \w     29.00 130.00   0.50    0.50    --   98.20 -61.00   0.00  202
 18  \w     31.00 188.00   0.50    0.50    --   98.20  15.00   0.00  314
 19  \w      9.00 130.00   0.50    0.50    --   98.20 -61.00 150.00  242
 20  \w     80.00 106.00   0.50    0.50    --   98.20 -82.00  90.00   52
 21  \w     15.00  58.00   0.50    0.50    --   98.20 -82.00  90.00   86
 22  \w     18.00  44.00   0.50    0.50    --   98.20 -61.00  30.00   52
 23  \w     80.00 105.00   0.50    0.50    --   98.20 -82.00 -90.00   50
 24  \w     43.00 188.00   0.50    0.50    --   98.20  15.00 -90.00  290
 25  \w     81.00 106.00   0.50    0.50    --   98.20 -82.00 -60.00   50
 26  \w     38.00 137.00   0.50    0.50    --   98.20 -82.00   0.00  198
 27  \w     89.00 127.00   0.50    0.50    --   98.20 -45.00 120.00   76
;
_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      -0.0939613000
_diffrn_orient_matrix_UB_12      -0.0115093000
_diffrn_orient_matrix_UB_13      -0.0756556000
_diffrn_orient_matrix_UB_21      -0.0610280000
_diffrn_orient_matrix_UB_22      0.0101608000
_diffrn_orient_matrix_UB_23      0.0532426000
_diffrn_orient_matrix_UB_31      0.0060680000
_diffrn_orient_matrix_UB_32      0.0974772000
_diffrn_orient_matrix_UB_33      0.0054611000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.994
_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       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42007
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.298
_diffrn_reflns_theta_min         1.878
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.886
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         15325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1375P)^2^+1.1374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12860
_reflns_number_total             15325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b04759_si_002.cif
_cod_data_source_block           1a
_cod_original_cell_volume        3933.10(18)
_cod_database_code               4514578
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOCd
_chemical_oxdiff_usercomment     z1007625
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.880
_reflns_odcompleteness_completeness 99.52
_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), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37),
 C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C48(H48), C49(H49), C50(H50),
  C51(H51), C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63),
 C64(H64), C65(H65)
;
_shelx_res_checksum              58959
_shelx_hkl_checksum              38896
_shelx_fab_checksum              39851
_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 2.214
_oxdiff_exptl_absorpt_empirical_full_min 0.600