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_4132893
_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
'C46 H35 Cl2 Co2 N6 O6, C6 H4 Cl2, 2(C F3 O3 S), 0.89(C6 Cl2), 0.12(Cl)'
_chemical_formula_sum            'C59.32 H39 Cl5.89 Co2 F6 N6 O12 S2'
_chemical_formula_weight         1532.58
_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             2018-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.155(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3260(5)
_cell_length_b                   25.5247(11)
_cell_length_c                   11.4411(5)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.29
_cell_measurement_theta_min      3.46
_cell_volume                     3014.9(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      99.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32366
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.642
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'INCOATEC Imus micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.128
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1330 before and 0.0979 after correction. The Ratio of minimum to maximum transmission is 0.4890. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       block
_exptl_crystal_F_000             1546
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 3442 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.148(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     909
_refine_ls_number_reflns         10964
_refine_ls_number_restraints     478
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0346P)^2^+11.3605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1461
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                9633
_reflns_number_total             10964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07290_si_002.cif
_cod_data_source_block           13R
_cod_database_code               4132893
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9424(14)
 0.0576(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 O7-H7
 0.87 with sigma of 0.01
 F7-C67 = F9-C67 = F8-C67
 1.35 with sigma of 0.02
 F9-F8
 2.11 with sigma of 0.02
 F9-F7
 2.11 with sigma of 0.02
 F8-F7
 2.11 with sigma of 0.02
 S3-C67
 1.8 with sigma of 0.02
 O3-H3
 0.9 with sigma of 0.02
 H3-H28
 -2.2 with sigma of 0.02
 F5-Cl2
 -3.22 with sigma of 0.02
 F7-C33
 -3.2 with sigma of 0.02
 C48-C47 = C47-C46 = C51-C46 = C51-C50 = C50-C49 = C49-C48
 1.39 with sigma of 0.01
 S2-C53
 1.8 with sigma of 0.02
 F4-C53 = F4-C53 = F4-C53
 1.358 with sigma of 0.02
 F5-C53 = F6-C53
 1.358 with sigma of 0.02
 Cl5A-C77 = Cl5B-C68 = Cl0A-C78 = Cl6-C73
 1.72 with sigma of 0.02
 Cl8-C85 = Cl7-C81
 1.72 with sigma of 0.02
 C1-H7
 1.91007 with sigma of 0.02
 Co1-H7
 2.826332 with sigma of 0.02
 S3-F8 \\sim S3-F9 \\sim S3-F7
 with sigma of 0.02
 S3-O8 \\sim S3-O13 \\sim S3-O17
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C73 \\sim Cl5B \\sim C68 \\sim C69 \\sim Cl6 \\sim C72 \\sim C70 \\sim C71
\\sim C80 \\sim Cl7 \\sim C81 \\sim C82 \\sim C85 \\sim C83 \\sim C84 \\sim Cl8
\\sim C76 \\sim Cl0A \\sim C78 \\sim C79 \\sim C77 \\sim C74 \\sim Cl5A \\sim
C75: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C53 \\sim S2 \\sim O8 \\sim O11 \\sim O12 \\sim S3 \\sim F4 \\sim F5 \\sim F6
\\sim O13 \\sim C67 \\sim O17 \\sim F7 \\sim F8 \\sim F9: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C53, S2, O8, O11, O12, S3, F4, F5, F6, O13, C67, O17, F7, F8, F9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(S2)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(O11)=Sof(O12)=Sof(C53)=1-FVAR(1)
 Sof(S3)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(O13)=Sof(C67)=Sof(O17)=FVAR(1)
 Sof(Cl5B)=Sof(Cl6)=Sof(C68)=Sof(C73)=Sof(C72)=Sof(C71)=Sof(C70)=Sof(C69)=
 FVAR(2)
 Sof(Cl0A)=Sof(C76)=Sof(C75)=Sof(C74)=Sof(C79)=Sof(C78)=Sof(C77)=Sof(Cl5A)=
 FVAR(3)
 Sof(Cl7)=Sof(C80)=Sof(C81)=Sof(C85)=Sof(C84)=Sof(C83)=Sof(C82)=Sof(Cl8)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C28(H28)
7.b Aromatic/amide H refined with riding coordinates:
 C7(H7A), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C40(H40), C42(H42), C44(H44), C45(H45), C46(H46),
  C47(H47), C50(H50), C51(H51), C54(H54)
7.c Fitted hexagon refined as free rotating group:
 C68(C73,C72,C71,C70,C69), C76(C75,C74,C79,C78,C77), C80(C81,C85,C84,C83,C82)
;
_olex2_submission_special_instructions 'No special instructions were received'