Soft Porous Crystal Based upon Organic Cages That Exhibit Guest-Induced Breathing and Selective Gas Separation.
Wang, Zhifang; Sikdar, Nivedita; Wang, Shi-Qiang; Li, Xia; Yu, Meihui; Bu, Xian-He; Chang, Ze; Zou, Xiaolong; Chen, Yao; Cheng, Peng; Yu, Kuang; Zaworotko, Michael J.; Zhang, Zhenjie; Journal of the American Chemical Society 141 (2019) 9408–9414; doi:10.1021/jacs.9b04319

data_4128749
_publ_section_title
;
 Soft Porous Crystal Based upon Organic Cages That Exhibit Guest-Induced
 Breathing and Selective Gas Separation.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9408
_journal_page_last               9414
_journal_paper_doi               10.1021/jacs.9b04319
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C60 H42 N8 O12, H2 O'
_chemical_formula_sum            'C60 H44 N8 O13'
_chemical_formula_weight         1085.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.318(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6187(15)
_cell_length_b                   15.7648(10)
_cell_length_c                   17.9841(11)
_cell_measurement_reflns_used    1756
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      21.4430
_cell_measurement_theta_min      3.1460
_cell_volume                     5136.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      1.00  85.00   0.75   42.50    --   18.78  57.00 -90.00  112
  2  \w    -54.00  -9.00   0.75   42.50    --  -20.03  19.00 120.00   60
  3  \w      9.00  52.50   0.75   42.50    --  -20.03  19.00 120.00   58
  4  \w    -40.00  25.25   0.75   42.50    --  -20.03  57.00-180.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0136059000
_diffrn_orient_matrix_UB_12      -0.0420620000
_diffrn_orient_matrix_UB_13      0.0059076000
_diffrn_orient_matrix_UB_21      -0.0340220000
_diffrn_orient_matrix_UB_22      -0.0132346000
_diffrn_orient_matrix_UB_23      0.0075703000
_diffrn_orient_matrix_UB_31      -0.0137483000
_diffrn_orient_matrix_UB_32      -0.0088653000
_diffrn_orient_matrix_UB_33      -0.0393969000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.1794
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19152
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.003
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         9030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1983
_refine_ls_R_factor_gt           0.0908
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.2233
_reflns_number_gt                4132
_reflns_number_total             9030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b04319_si_002.cif
_cod_data_source_block           NKPOC-1-alfa
_cod_database_code               4128749
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O13(H13A,H13B)
2.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C21(H21A,H21B), C39(H39A,H39B), C41(H41A,H41B), C2(H2A,H2B),
 C22(H22A,H22B), C59(H59A,H59B), C1(H1A,H1B), C60(H60A,H60B), C19(H19A,H19B),
 C20(H20A,H20B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C12(H12), C13(H13), C7(H7), C29(H29), C14(H14), C34(H34), C48(H48),
 C28(H28), C27(H27), C49(H49), C9(H9), C53(H53), C52(H52), C47(H47), C8(H8),
 C54(H54), C32(H32)
;
_olex2_date_sample_data_collection 2018-12-24
_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 1.559
_oxdiff_exptl_absorpt_empirical_full_min 0.550