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_4132897
_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 H36 Cl2 Co2 N6 O6, 2(C F3 O3 S), C7 H5 F3, 2(C H4 O)'
_chemical_formula_sum            'C57 H49 Cl2 Co2 F9 N6 O14 S2'
_chemical_formula_weight         1465.90
_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                 90.213(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1640(6)
_cell_length_b                   25.6088(15)
_cell_length_c                   11.4722(7)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.49
_cell_measurement_theta_min      3.45
_cell_volume                     2986.1(3)
_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      100.22
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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  0.0660
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            40517
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.772
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'INCOATEC Imus micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.708
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1318 before and 0.1017 after correction. The Ratio of minimum to maximum transmission is 0.6436. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 3837 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.041(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         11478
_refine_ls_number_restraints     494
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0290P)^2^+3.2140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                9998
_reflns_number_total             11478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07290_si_003.cif
_cod_data_source_block           33R
_cod_database_code               4132897
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.637
_shelx_estimated_absorpt_t_min   0.443
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5745(16)
 0.4255(16)
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
 F8-C50 = F7-C50 = F9-C50
 1.323 with sigma of 0.02
 F12-C58 = F11-C58 = F10-C58
 1.323 with sigma of 0.02
 O6-H6
 0.87 with sigma of 0.02
 O4-H4
 0.87 with sigma of 0.02
 H4-C15
 1.92 with sigma of 0.02
 C40-H6
 1.92 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
F7 \\sim C50 \\sim F8 \\sim F9 \\sim C54 \\sim C53 \\sim C55 \\sim C52 \\sim
C56 \\sim C51 \\sim C61 \\sim F10 \\sim C58 \\sim F11 \\sim F12 \\sim C64 \\sim
C59 \\sim C63 \\sim C60 \\sim C62: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C57 \\sim O14: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 F7, C50, F8, F9, C54, C53, C55, C52, C56, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C60, F10, C58, F11, F12, C64, C59, C63, C62, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C57, O14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=
 Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C53)=
 Sof(H53)=Sof(C54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C15(H15), C40(H40)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5), C6(H6A), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C29(H29), C30(H30), C32(H32), C33(H33), C36(H36),
 C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C59(H59),
 C60(H60), C61(H61), C62(H62), C63(H63)
7.c Fitted hexagon refined as free rotating group:
 C51(C52,C53,C54,C55,C56), C59(C60,C61,C62,C63,C64)
7.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C57(H57A,H57B,H57C)
7.e Idealised tetrahedral OH refined as rotating group:
 O13(H13A), O14(H14A)
;
_olex2_submission_special_instructions 'No special instructions were received'