High temperature expulsion of thermolabile groups for pore-space expansion in metal‒organic frameworks
Bryant, Macguire R.; Ablott, Timothy A.; Telfer, Shane G.; Liu, Lujia; Richardson, Christopher; CrystEngComm 21 (2019) 60–; doi:10.1039/C8CE01740A

data_7231779
_publ_section_title
;
 High temperature expulsion of thermolabile groups for pore-space
 expansion in metal--organic frameworks
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              60
_journal_paper_doi               10.1039/C8CE01740A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C48 H30 O13 Zn4, 0.5(H2 O)'
_chemical_formula_sum            'C48 H31 O13.5 Zn4'
_chemical_formula_weight         1085.21
_chemical_name_common            WUF-19
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2018-10-11 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.869(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.47(2)
_cell_length_b                   24.029(17)
_cell_length_c                   17.149(12)
_cell_measurement_reflns_used    327
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      46
_cell_measurement_theta_min      2.6
_cell_volume                     10082(13)
_computing_cell_refinement       'FSProcess in Process-Auto (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess in Process-Auto (Rigaku, 1998)'
_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      292
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Osmic optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1675
_diffrn_reflns_av_unetI/netI     0.1437
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11545
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        36.348
_diffrn_reflns_theta_max         36.348
_diffrn_reflns_theta_min         5.729
_diffrn_source                   'Rigaku MM007 rotating anode'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    0.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.943
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.771
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2365
_refine_ls_number_restraints     473
_refine_ls_restrained_S_all      2.566
_refine_ls_R_factor_all          0.2370
_refine_ls_R_factor_gt           0.1810
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4599
_refine_ls_wR_factor_ref         0.4986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1402
_reflns_number_total             2365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01740a2.cif
_cod_data_source_block           mb5071b
_cod_depositor_comments          'Adding full bibliography for 7231779.cif.'
_cod_original_formula_sum        'C48 H31 O13.50 Zn4'
_cod_database_code               7231779
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H70 of C70, H26 of C26, H30 of C30, H34 of C34, H21 of
  C21, H12 of C12, H15 of C15, H22 of C22, H33 of C33, H31 of C31, H13 of C13,
  H19 of C19, H16 of C16
 At 1.5 times of:
  All C(H,H,H) groups, H27 of C71, All O(H) groups
2. Restrained distances
 C34-C28
 2.4 with sigma of 0.04
 O41-C23_$1 \\sim O24-C24 \\sim O37-C35 \\sim O36-C35
 with sigma of 0.02
 C23-C20 \\sim C11-C10 \\sim C35-C32 \\sim C25-C24
 with sigma of 0.02
 C34-C29 \\sim C30-C29
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H50(0.5) C70(0.5) H70(0.5) C71(0.5) H27(0.5) H71A(0.5) H71B(0.5)
 Fixed Uiso: C60(0.2) C61(0.2) C70(0.2) C71(0.2)
 Fixed X: C60(0.867001) C61(0.820001) H60(0.878) H61A(0.796) H61B(0.805)
 C70(0.641001) C71(0.642) H27(0.654) H71A(0.63558) H71B(0.64906)
 Fixed Y: C60(0.822001) C61(0.796) H60(0.852) H61A(0.805) H61B(0.767)
 C70(0.602) C71(0.618001) H27(0.582) H71A(0.652121) H71B(0.59413)
 Fixed Z: C60(0.127001) C61(0.115001) H60(0.084) H61A(0.065001) H61B(0.156)
 C70(0.693001) C71(0.768001) H27(0.698001) H71A(0.77992) H71B(0.80414)
6.a Riding coordinates:
 O50(H50)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C21(H21), C22(H22), C19(H19),
 C26(H26), C30(H30), C31(H31), C33(H33), C34(H34), C70(H70)
6.c Fitted hexagon refined as free rotating group:
 C11(C12,C13,C14,C15,C16), C20(C21,C22,C17,C18,C19)
;
_olex2_submission_special_instructions 'No special instructions were received'