Modulation of Water Vapor Sorption by a Fourth-Generation Metal-Organic Material with a Rigid Framework and Self-Switching Pores.
Zhang, Shi-Yuan; Jensen, Stephanie; Tan, Kui; Wojtas, Lukasz; Roveto, Matthew; Cure, Jeremy; Thonhauser, Timo; Chabal, Yves J.; Zaworotko, Michael J.; Journal of the American Chemical Society 140 (2018) 12545–12552; doi:10.1021/jacs.8b07290

data_4132896
_publ_section_title
;
 Modulation of Water Vapor Sorption by a Fourth-Generation Metal-Organic
 Material with a Rigid Framework and Self-Switching Pores.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12545
_journal_page_last               12552
_journal_paper_doi               10.1021/jacs.8b07290
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C48 H42 Co2 N6 O6, 2(C F3 O3 S), 1(C7 H5 F3), 2(C H4 O)'
_chemical_formula_sum            'C59 H55 Co2 F9 N6 O14 S2'
_chemical_formula_weight         1425.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4539(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1791(3)
_cell_length_b                   25.6037(8)
_cell_length_c                   11.4781(4)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.25
_cell_measurement_theta_min      3.85
_cell_volume                     2991.36(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.34
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34091
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.584
_diffrn_reflns_theta_min         3.452
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.874
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.1393 before and 0.1031 after correction. The Ratio of minimum to maximum transmission is 0.6359. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 3717 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.155(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         11404
_refine_ls_number_restraints     482
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0634
_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^)+8.5113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                10256
_reflns_number_total             11404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07290_si_004.cif
_cod_data_source_block           43R
_cod_database_code               4132896
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.651
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8913(17)
 0.1087(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 O14-C52
 1.44 with sigma of 0.02
 F8-F7
 2.11 with sigma of 0.02
 F7-F9
 2.11 with sigma of 0.02
 F9-F8
 2.11 with sigma of 0.02
 F8-C53 = F7-C53 = F9-C53
 1.323 with sigma of 0.02
 F10-F11
 2.11 with sigma of 0.02
 F11-F12
 2.11 with sigma of 0.02
 F10-F12
 2.11 with sigma of 0.02
 F10-C60 = F11-C60 = F12-C60
 1.323 with sigma of 0.02
 F14-C67 = F15-C67 = F13-C67
 1.323 with sigma of 0.02
 F15-F14
 2.11 with sigma of 0.02
 F15-F13
 2.11 with sigma of 0.02
 F13-F14
 2.11 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C59 \\sim F10 \\sim C60 \\sim F11 \\sim F12 \\sim C58 \\sim C57 \\sim C56 \\sim
C54 \\sim C55 \\sim C64 \\sim F13 \\sim C67 \\sim F14 \\sim F15 \\sim C63 \\sim
C62 \\sim C61 \\sim C65 \\sim C66: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C64, F13, C67, F14, F15, C63, C62, C61, C65, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, F10, C60, F11, F12, C58, C57, C56, C54, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=
 Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=
 Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(C59)=Sof(H59)=Sof(C60)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C21(H21), C22(H22)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C23(H23), C24(H24),
  C25(H25), C27(H27), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48),
  C49(H49), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C61(H61),
 C62(H62), C64(H64), C65(H65), C66(H66)
7.c Fitted hexagon refined as free rotating group:
 C54(C55,C56,C57,C58,C59), C61(C62,C63,C64,C65,C66)
7.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C)
7.e Idealised tetrahedral OH refined as rotating group:
 O13(H13), O14(H14A)
;
_olex2_submission_special_instructions 'No special instructions were received'