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_4514577
_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 H81 Cd4 N32 O16'
_chemical_formula_sum            'C128 H81 Cd4 N32 O16'
_chemical_formula_weight         2772.84
_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
_atom_sites_solution_primary     dual
_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                76.6130(10)
_cell_angle_beta                 78.7810(10)
_cell_angle_gamma                74.3780(10)
_cell_formula_units_Z            2
_cell_length_a                   15.4922(2)
_cell_length_b                   17.7766(2)
_cell_length_c                   29.2303(4)
_cell_measurement_reflns_used    44283
_cell_measurement_temperature    298.3(2)
_cell_measurement_theta_max      74.0530
_cell_measurement_theta_min      4.0150
_cell_volume                     7466.49(17)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.3(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            89252
_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         74.867
_diffrn_reflns_theta_min         3.488
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_exptl_absorpt_coefficient_mu    5.035
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48538
_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    1.233
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             2786
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.455
_refine_diff_density_min         -1.765
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1597
_refine_ls_number_reflns         29414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1130P)^2^+1.3674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24105
_reflns_number_total             29414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b04759_si_004.cif
_cod_data_source_block           1b
_cod_database_code               4514577
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.464
_shelx_estimated_absorpt_t_min   0.378
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N11(H11), C1(H1), C2(H2), C4(H4), C5(H5), C10(H10), C11(H11A), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C28(H28), C29(H29), C31(H31), C30(H30), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C46(H46), C47(H47),
  C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55),
 C58(H58), C59(H59), C61(H61), C66(H66), C67(H67), C69(H69), C68(H68), C71(H71),
  C72(H72), C73(H73), C74(H74), C77(H77), C78(H78), C80(H80), C81(H81),
 C83(H83), C84(H84), C86(H86), C87(H87), C91(H91), C92(H92), C94(H94), C95(H95),
  C97(H97), C98(H98), C100(H100), C101(H101), C105(H105), C106(H106),
 C108(H108), C109(H109), C111(H111), C112(H112), C114(H114), C115(H115),
 C119(H119), C120(H120), C121(H121), C122(H122), C125(H125), C126(H126),
 C128(H128), C129(H129)
2.b Fitted hexagon refined as free rotating group:
 C27(C28,C29,N16,C31,C30), C65(C66,C67,N32,C69,C68)
;
_shelx_res_checksum              62687
_shelx_hkl_checksum              15233
_shelx_fab_checksum              81096
_olex2_submission_special_instructions 'No special instructions were received'