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_4132894
_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 ad
_chemical_formula_moiety
'C46 H38 Co2 N6 O6, 1.9(C6 H4 Cl2), 2(C F3 O3 S)'
_chemical_formula_sum            'C59.42 H45.61 Cl3.81 Co2 F6 N6 O12 S2'
_chemical_formula_weight         1466.48
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.403(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3499(5)
_cell_length_b                   25.4610(12)
_cell_length_c                   11.4211(6)
_cell_measurement_temperature    100(2)
_cell_volume                     3008.8(3)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            37053
_diffrn_reflns_theta_full        65.23
_diffrn_reflns_theta_max         65.23
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.281
_exptl_absorpt_correction_T_max  0.9308
_exptl_absorpt_correction_T_min  0.7123
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1490
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.048(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         9634
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+8.7525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                8763
_reflns_number_total             9634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b07290_si_006.cif
_cod_data_source_block           3S
_cod_database_code               4132894
_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) groups
2. Restrained distances
 O4-H4
 0.88 with sigma of 0.02
 O6-H6
 0.88 with sigma of 0.02
 H33-H4
 -2.2 with sigma of 0.02
 H8A-H6
 -2.2 with sigma of 0.02
 C45-C43 = C50-C45 = C54-C50 = C54-C52 = C52-C51 = C51-C43
 1.39 with sigma of 0.01
 H4-C33
 1.89 with sigma of 0.04
 H6-C8
 1.9 with sigma of 0.04
 Cl4-C56 \\sim Cl6-C61 \\sim Cl3-C55 \\sim Cl5-C62
 with sigma of 0.01
 C8-C20B \\sim C8-C20A
 with sigma of 0.01
3. Rigid bond restraints
 C61, C66, C65, C64, C63, C62
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl6, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C46B, C49B, C48B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C55 \\sim C61 \\sim C66 \\sim C56 \\sim C57 \\sim C65 \\sim C64 \\sim C58 \\sim
C63 \\sim C59 \\sim C62 \\sim C60: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Cl6 \\sim Cl3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C61 \\sim C55: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Sof(Cl5)=Sof(Cl6)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C55)=Sof(C56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=
 Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=FVAR(2)
 Sof(H8A)=1-FVAR(3)
 Sof(H8B)=Sof(Cl1)=Sof(Cl2)=Sof(C43)=Sof(C45)=Sof(C50)=Sof(H50)=Sof(C51)=
 Sof(H51)=Sof(C52)=Sof(H52)=Sof(C54)=Sof(H54)=FVAR(3)
 Fixed Sof: C20B(0.6) C37A(0.6) H37A(0.6) C46A(0.6) H46A(0.6) C49A(0.6)
 H49A(0.6) C48A(0.6) H48A(0.6) C40A(0.6) H40A(0.6) C20A(0.4) C40B(0.4)
 H40B(0.4) C48B(0.4) H48B(0.4) C49B(0.4) H49B(0.4) C46B(0.4) H46B(0.4)
 C37B(0.4) H37B(0.4)
6.a Ternary CH refined with riding coordinates:
 C8(H8A), C8(H8B), C33(H33)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6A), C7(H7), C9(H9), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C37A(H37A), C46A(H46A), C49A(H49A),
 C48A(H48A), C40A(H40A), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27),
 C28(H28), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C38(H38),
  C39(H39), C41(H41), C42(H42), C44(H44), C50(H50), C51(H51), C52(H52),
 C54(H54), C57(H57), C58(H58), C59(H59), C60(H60), C63(H63), C64(H64), C65(H65),
  C66(H66), C40B(H40B), C48B(H48B), C49B(H49B), C46B(H46B), C37B(H37B)
6.c Fitted hexagon refined as free rotating group:
 C20B(C37A,C46A,C49A,C48A,C40A), C55(C56,C57,C58,C59,C60), C61(C62,C63,C64,C65,
 C66), C20A(C40B,C48B,C49B,C46B,C37B)
;
_olex2_submission_special_instructions 'No special instructions were received'