Visualizing Structural Transformation and Guest Binding in a Flexible Metal-Organic Framework under High Pressure and Room Temperature.
Yang, Hui; Guo, Feng; Lama, Prem; Gao, Wen-Yang; Wu, Hui; Barbour, Leonard J.; Zhou, Wei; Zhang, Jian; Aguila, Briana; Ma, Shengqian; ACS central science 4 (2018) 1194–1200; doi:10.1021/acscentsci.8b00378

data_4515846
_publ_section_title
;
 Visualizing Structural Transformation and Guest Binding in a Flexible
 Metal-Organic Framework under High Pressure and Room Temperature.
;
_journal_issue                   9
_journal_name_full               'ACS central science'
_journal_page_first              1194
_journal_page_last               1200
_journal_paper_doi               10.1021/acscentsci.8b00378
_journal_volume                  4
_journal_year                    2018
_chemical_formula_moiety         '0.25(C88 H72 Cd4 N16 O16)'
_chemical_formula_sum            'C22 H18 Cd N4 O4'
_chemical_formula_weight         514.80
_space_group_crystal_system      tetragonal
_space_group_IT_number           90
_space_group_name_Hall           'P 4ab 2ab'
_space_group_name_H-M_alt        'P 4 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.21 svn.r3092 for OlexSys, GUI svn.r4949)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.636(3)
_cell_length_b                   18.636(3)
_cell_length_c                   8.2243(15)
_cell_measurement_reflns_used    4093
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.32
_cell_measurement_theta_min      2.44
_cell_volume                     2856.3(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 venture PHOTON II CPAD'
_diffrn_measurement_method       '\f \ch and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            30437
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.186
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  0.089
_exptl_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.252
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 603 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2510
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+12.7130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1794
_refine_ls_wR_factor_ref         0.1935
_reflns_Friedel_coverage         0.690
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                1953
_reflns_number_total             2510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc8b00378_si_005.cif
_cod_data_source_block           20barCO2_sq
_cod_original_cell_volume        2856.2(11)
_cod_database_code               4515846
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.873
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C11
 1.48 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.015 and sigma for
terminal atoms of 0.03
4. Others
 Fixed X: O1(0.38234) C11(0.363301)
 Fixed Y: O1(0.263981) C11(0.242229)
 Fixed Z: O1(0.09936) C11(0.23728)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C9(H9), C10(H10)
5.b Fitted pentagon refined as free rotating group:
 N1(C1,C2,N2,C3)
5.c Fitted hexagon refined as free rotating group:
 C5(C6,C7,C8,C9,C10)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              55240
_shelx_hkl_checksum              25192
_shelx_fab_checksum              89604
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'