Ultraporous, Water Stable, and Breathing Zirconium-Based Metal-Organic Frameworks with ftw Topology.
Deria, Pravas; Gómez-Gualdrón, Diego A; Bury, Wojciech; Schaef, Herbert T.; Wang, Timothy C.; Thallapally, Praveen K.; Sarjeant, Amy A.; Snurr, Randall Q.; Hupp, Joseph T.; Farha, Omar K.; Journal of the American Chemical Society 137 (2015) 13183–13190; doi:10.1021/jacs.5b08860

data_4129624
_publ_section_title
;
 Ultraporous, Water Stable, and Breathing Zirconium-Based Metal-Organic
 Frameworks with ftw Topology.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13183
_journal_page_last               13190
_journal_paper_doi               10.1021/jacs.5b08860
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C312 H210 O32 Zr6'
_chemical_formula_sum            'C312 H210 O32 Zr6'
_chemical_formula_weight         5018.11
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.11 svn.r2872 for OlexSys, GUI svn.r4767)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   30.1088(11)
_cell_length_b                   30.1088(11)
_cell_length_c                   30.1088(11)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      67.501
_cell_measurement_theta_min      3.282
_cell_volume                     27294.8(17)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            314615
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.305
_diffrn_reflns_theta_min         1.467
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.6953
_exptl_absorpt_correction_T_min  0.6359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1019 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.9146.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.305
_exptl_crystal_description       block
_exptl_crystal_F_000             2578
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.561
_refine_diff_density_min         -1.549
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4807
_refine_ls_number_restraints     8985
_refine_ls_restrained_S_all      0.827
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1567P)^2^+6.6084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2200
_refine_ls_wR_factor_ref         0.2291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4318
_reflns_number_total             4807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08860_si_002.cif
_cod_data_source_block           n3257_a
_cod_original_cell_volume        27295(3)
_cod_database_code               4129624
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C221-C222 = C122-C121 = C422-C421 = C322-C321
 2.154 with sigma of 0.001
 C402-C101_$1
 1.542 with sigma of 0.02
 C202-C101_$2
 1.542 with sigma of 0.02
 C101_$3-C302
 1.542 with sigma of 0.02
 C101-C102 \\sim C105-C108 \\sim C1-C117 \\sim C205-C208 \\sim C3-C217 \\sim
C417-C10 \\sim C405-C408
 \\sim C305-C308 \\sim C317-C8 \\sim C402-C101_$1 \\sim C202-C101_$2 \\sim
C101_$3-C302
 with sigma of 0.02
 C120-C119 \\sim C120-C112 \\sim C122-C120 \\sim C121-C120 \\sim C220-C219
\\sim C220-C212 \\sim C222-
 C220 \\sim C221-C220 \\sim C320-C319 \\sim C320-C312 \\sim C321-C320 \\sim
C322-C320 \\sim C420-C419 -
 C422-C420 \\sim C421-C420 \\sim C420-C412
 with sigma of 0.02
 C121-C122 \\sim C221-C222 \\sim C321-C322 \\sim C422-C421
 with sigma of 0.02
 C107-C102 \\sim C107-C106 \\sim C106-C105 \\sim C105-C104 \\sim C104-C103
\\sim C103-C102 \\sim C109-
 C108 \\sim C110-C109 \\sim C111-C110 \\sim C112-C111 \\sim C113-C112 \\sim
C113-C108 \\sim C115-C114 -
 C116-C115 \\sim C117-C116 \\sim C118-C117 \\sim C119-C118 \\sim C119-C114
\\sim C203-C202 \\sim C204-
 C203 \\sim C205-C204 \\sim C206-C205 \\sim C207-C206 \\sim C207-C202 \\sim
C213-C208 \\sim C213-C212 -
 C212-C211 \\sim C211-C210 \\sim C210-C209 \\sim C209-C208 \\sim C219-C214
\\sim C219-C218 \\sim C218-
 C217 \\sim C217-C216 \\sim C216-C215 \\sim C215-C214 \\sim C307-C302 \\sim
C307-C306 \\sim C306-C305 -
 C305-C304 \\sim C304-C303 \\sim C303-C302 \\sim C309-C308 \\sim C310-C309
\\sim C311-C310 \\sim C312-
 C311 \\sim C313-C312 \\sim C313-C308 \\sim C315-C314 \\sim C316-C315 \\sim
C317-C316 \\sim C318-C317 -
 C319-C318 \\sim C319-C314 \\sim C407-C402 \\sim C403-C402 \\sim C404-C403
\\sim C405-C404 \\sim C406-
 C405 \\sim C407-C406 \\sim C413-C408 \\sim C413-C412 \\sim C412-C411 \\sim
C411-C410 \\sim C410-C409 -
 C409-C408 \\sim C419-C414 \\sim C419-C418 \\sim C418-C417 \\sim C417-C416
\\sim C416-C415 \\sim C415-
 C414 \\sim C2-C1 \\sim C3-C2 \\sim C4-C3 \\sim C5-C4 \\sim C6-C5 \\sim C7-C6
\\sim C8-C7 \\sim C9-C8 \\sim C9-C10
 \\sim C11-C10 \\sim C12-C11 \\sim C13-C12 \\sim C14-C13 \\sim C14-C1 \\sim
C15-C14 \\sim C4-C15 \\sim C16-C15
 \\sim C7-C16 \\sim C16-C11
 with sigma of 0.02
 C102-C105 \\sim C107-C104 \\sim C106-C103 \\sim C108-C111 \\sim C109-C112
\\sim C110-C113 \\sim C114-
 C117 \\sim C115-C118 \\sim C116-C119 \\sim C202-C205 \\sim C203-C206 \\sim
C207-C204 \\sim C208-C211 -
 C213-C210 \\sim C209-C212 \\sim C214-C217 \\sim C219-C216 \\sim C218-C215
\\sim C302-C305 \\sim C307-
 C304 \\sim C306-C303 \\sim C308-C311 \\sim C309-C312 \\sim C310-C313 \\sim
C314-C317 \\sim C315-C318 -
 C316-C319 \\sim C402-C405 \\sim C403-C406 \\sim C404-C407 \\sim C408-C411
\\sim C413-C410 \\sim C412-
 C409 \\sim C414-C417 \\sim C419-C416 \\sim C418-C415
 with sigma of 0.02
 C1-C4 \\sim C2-C15 \\sim C3-C14 \\sim C10-C7 \\sim C9-C16 \\sim C8-C11 \\sim
C12-C15 \\sim C13-C16 \\sim C11-
 C14 \\sim C15-C6 \\sim C16-C5 \\sim C7-C4
 with sigma of 0.02
 C114-C111 \\sim C214-C211 \\sim C314-C311 \\sim C414-C411
 with sigma of 0.02
 C102-C106 \\sim C107-C105 \\sim C108-C110 \\sim C109-C111 \\sim C114-C116
\\sim C115-C117 \\sim C202-
 C204 \\sim C203-C205 \\sim C208-C212 \\sim C213-C211 \\sim C214-C218 \\sim
C219-C217 \\sim C302-C306 -
 C307-C305 \\sim C308-C310 \\sim C309-C311 \\sim C314-C316 \\sim C315-C317
\\sim C402-C404 \\sim C403-
 C405 \\sim C408-C412 \\sim C413-C411 \\sim C414-C418 \\sim C419-C417 \\sim
C102-C104 \\sim C103-C105 -
 C108-C112 \\sim C113-C111 \\sim C114-C118 \\sim C119-C117 \\sim C202-C206
\\sim C207-C205 \\sim C208-
 C210 \\sim C209-C211 \\sim C214-C216 \\sim C215-C217 \\sim C302-C304 \\sim
C303-C305 \\sim C308-C312 -
 C313-C311 \\sim C314-C318 \\sim C319-C317 \\sim C402-C406 \\sim C407-C405
\\sim C408-C410 \\sim C409-
 C411 \\sim C414-C416 \\sim C415-C417 \\sim C107-C103 \\sim C106-C104 \\sim
C109-C113 \\sim C110-C112 -
 C115-C119 \\sim C116-C118 \\sim C207-C203 \\sim C206-C204 \\sim C209-C213
\\sim C210-C212 \\sim C215-
 C219 \\sim C216-C218 \\sim C303-C307 \\sim C304-C306 \\sim C313-C309 \\sim
C312-C310 \\sim C319-C315 -
 C318-C316 \\sim C403-C407 \\sim C404-C406 \\sim C413-C409 \\sim C412-C410
\\sim C419-C415 \\sim C418-
 C416
 with sigma of 0.02
 C1-C3 \\sim C2-C4 \\sim C5-C7 \\sim C6-C16 \\sim C8-C10 \\sim C9-C11 \\sim
C12-C14 \\sim C13-C15
 with sigma of 0.02
 C121-C112 \\sim C122-C119 \\sim C222-C212 \\sim C221-C219 \\sim C321-C312
\\sim C322-C319 \\sim C421-
 C412 \\sim C422-C419 \\sim C121-C119 \\sim C122-C112 \\sim C222-C219 \\sim
C221-C212 \\sim C321-C319 -
 C322-C312 \\sim C421-C419 \\sim C422-C412
 with sigma of 0.02
 C112-C114 \\sim C111-C119 \\sim C212-C214 \\sim C211-C219 \\sim C312-C314
\\sim C311-C319 \\sim C412-
 C414 \\sim C411-C419 \\sim C112-C119 \\sim C120-C114 \\sim C212-C219 \\sim
C220-C214 \\sim C312-C319 -
 C320-C314 \\sim C412-C419 \\sim C420-C414 \\sim C120-C111 \\sim C220-C211
\\sim C320-C311 \\sim C420-
 C411
 with sigma of 0.02
 C101-C103 \\sim C101-C107 \\sim C101_$1-C403 \\sim C101_$1-C407 \\sim
C101_$2-C203 \\sim C101_$2-
 C207 \\sim C101_$3-C303 \\sim C101_$3-C307
 with sigma of 0.02
 C104-C108 \\sim C106-C108 \\sim C204-C208 \\sim C206-C208 \\sim C304-C308
\\sim C306-C308 \\sim C404-
 C408 \\sim C406-C408
 with sigma of 0.02
3. Restrained planarity
 C14, C15, C13, C12, C11, C16, C7, C10, C9, C8, C3, C2, C1, C4, C6, C5, C117,
 C217, C317, C417
 with sigma of 0.01
 C108, C105, C106, C107, C102, C103, C104, C101
 with sigma of 0.1
 C116, C115, C114, C119, C118, C111, C112, C113, C108, C109, C110, C120, C117,
 C1, C105
 with sigma of 0.1
 C205, C206, C207, C202, C203, C204, C208
 with sigma of 0.1
 C3, C217, C216, C215, C214, C219, C218, C211, C212, C213, C208, C209, C210,
 C220, C205
 with sigma of 0.1
 C105, C106, C107, C102, C103, C104, C101, C108
 with sigma of 0.1
 C305, C304, C303, C302, C307, C306, C308
 with sigma of 0.1
 C317, C318, C319, C314, C315, C316, C311, C310, C309, C308, C313, C312, C320,
 C305, C8
 with sigma of 0.1
 C405, C404, C403, C402, C407, C406, C408
 with sigma of 0.1
 C410, C417, C418, C419, C414, C415, C416, C411, C409, C408, C413, C412, C420,
 C405, C10
 with sigma of 0.1
 C208, C205, C206, C207, C202, C203, C204
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(C14) = Uanis(C15) = Uanis(C4) =
Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C16) = Uanis(C7) = Uanis(C6) =
Uanis(C5) = Uanis(C10) = Uanis(C9) = Uanis(C8) = Uanis(C217) = Uanis(C117) =
Uanis(C417) = Uanis(C317) = Uanis(C216) = Uanis(C215) = Uanis(C214) =
Uanis(C219) = Uanis(C218) = Uanis(C318) = Uanis(C319) = Uanis(C314) =
Uanis(C315) = Uanis(C316) = Uanis(C116) = Uanis(C115) = Uanis(C114) =
Uanis(C119) = Uanis(C118) = Uanis(C418) = Uanis(C419) = Uanis(C414) =
Uanis(C415) = Uanis(C416) = Uanis(C211) = Uanis(C311) = Uanis(C111) =
Uanis(C411) = Uanis(C212) = Uanis(C213) = Uanis(C208) = Uanis(C209) =
Uanis(C210) = Uanis(C112) = Uanis(C113) = Uanis(C108) = Uanis(C109) =
Uanis(C110) = Uanis(C310) = Uanis(C309) = Uanis(C308) = Uanis(C313) =
Uanis(C312) = Uanis(C410) = Uanis(C409) = Uanis(C408) = Uanis(C413) =
Uanis(C412) = Uanis(C205) = Uanis(C105) = Uanis(C305) = Uanis(C405) =
Uanis(C206) = Uanis(C207) = Uanis(C202) = Uanis(C203) = Uanis(C204) =
Uanis(C304) = Uanis(C303) = Uanis(C302) = Uanis(C307) = Uanis(C306) =
Uanis(C106) = Uanis(C107) = Uanis(C102) = Uanis(C103) = Uanis(C104) =
Uanis(C404) = Uanis(C403) = Uanis(C402) = Uanis(C407) = Uanis(C406) =
Uanis(C220) = Uanis(C320) = Uanis(C120) = Uanis(C420) = Uanis(C101) =
Uanis(C421) = Uanis(C422) = Uanis(C121) = Uanis(C122) = Uanis(C222) =
Uanis(C221) = Uanis(C321) = Uanis(C322)
5. 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
6. Others
 Fixed Sof: C1(0.0625) C2(0.0625) H2(0.0625) C3(0.0625) C4(0.0625) C5(0.0625)
 H5(0.0625) C6(0.0625) H6(0.0625) C7(0.0625) C8(0.0625) C9(0.0625) H9(0.0625)
 C10(0.0625) C11(0.0625) C12(0.0625) H12(0.0625) C13(0.0625) H13(0.0625)
 C14(0.0625) C15(0.0625) C16(0.0625) C102(0.0625) C103(0.0625) H103(0.0625)
 C104(0.0625) H104(0.0625) C105(0.0625) C106(0.0625) H106(0.0625) C107(0.0625)
 H107(0.0625) C108(0.0625) C109(0.0625) H109(0.0625) C110(0.0625) H110(0.0625)
 C111(0.0625) C112(0.0625) C113(0.0625) H113(0.0625) C114(0.0625) C115(0.0625)
 H115(0.0625) C116(0.0625) H116(0.0625) C117(0.0625) C118(0.0625) H118(0.0625)
 C119(0.0625) C120(0.0625) C121(0.0625) H12A(0.0625) H12B(0.0625) H12C(0.0625)
 C122(0.0625) H12D(0.0625) H12E(0.0625) H12F(0.0625) C202(0.0625) C203(0.0625)
 H203(0.0625) C204(0.0625) H204(0.0625) C205(0.0625) C206(0.0625) H206(0.0625)
 C207(0.0625) H207(0.0625) C208(0.0625) C209(0.0625) H209(0.0625) C210(0.0625)
 H210(0.0625) C211(0.0625) C212(0.0625) C213(0.0625) H213(0.0625) C214(0.0625)
 C215(0.0625) H215(0.0625) C216(0.0625) H216(0.0625) C217(0.0625) C218(0.0625)
 H218(0.0625) C219(0.0625) C220(0.0625) C221(0.0625) H22A(0.0625) H22B(0.0625)
 H22C(0.0625) C222(0.0625) H22D(0.0625) H22E(0.0625) H22F(0.0625) C302(0.0625)
 C303(0.0625) H303(0.0625) C304(0.0625) H304(0.0625) C305(0.0625) C306(0.0625)
 H306(0.0625) C307(0.0625) H307(0.0625) C308(0.0625) C309(0.0625) H309(0.0625)
 C310(0.0625) H310(0.0625) C311(0.0625) C312(0.0625) C313(0.0625) H313(0.0625)
 C314(0.0625) C315(0.0625) H315(0.0625) C316(0.0625) H316(0.0625) C317(0.0625)
 C318(0.0625) H318(0.0625) C319(0.0625) C320(0.0625) C321(0.0625) H32A(0.0625)
 H32B(0.0625) H32C(0.0625) C322(0.0625) H32D(0.0625) H32E(0.0625) H32F(0.0625)
 C402(0.0625) C403(0.0625) H403(0.0625) C404(0.0625) H404(0.0625) C405(0.0625)
 C406(0.0625) H406(0.0625) C407(0.0625) H407(0.0625) C408(0.0625) C409(0.0625)
 H409(0.0625) C410(0.0625) H410(0.0625) C411(0.0625) C412(0.0625) C413(0.0625)
 H413(0.0625) C414(0.0625) C415(0.0625) H415(0.0625) C416(0.0625) H416(0.0625)
 C417(0.0625) C418(0.0625) H418(0.0625) C419(0.0625) C420(0.0625) C421(0.0625)
 H42A(0.0625) H42B(0.0625) H42C(0.0625) C422(0.0625) H42D(0.0625) H42E(0.0625)
 H42F(0.0625)
7.a Riding coordinates:
 C222(H22D,H22E,H22F)
7.b Me refined with riding coordinates:
 C121(H12A,H12B,H12C), C122(H12D,H12E,H12F), C221(H22A,H22B,H22C), C321(H32A,
 H32B,H32C), C322(H32D,H32E,H32F), C421(H42A,H42B,H42C), C422(H42D,H42E,H42F)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C9(H9), C12(H12), C13(H13), C103(H103), C104(H104),
 C106(H106), C107(H107), C109(H109), C110(H110), C113(H113), C115(H115),
 C116(H116), C118(H118), C203(H203), C204(H204), C206(H206), C207(H207),
 C209(H209), C210(H210), C213(H213), C215(H215), C216(H216), C218(H218),
 C303(H303), C304(H304), C306(H306), C307(H307), C309(H309), C310(H310),
 C313(H313), C315(H315), C316(H316), C318(H318), C403(H403), C404(H404),
 C406(H406), C407(H407), C409(H409), C410(H410), C413(H413), C415(H415),
 C416(H416), C418(H418)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 18469.9 Ang^3^ [67.7%]
Total electron count / cell = 1887.8
;
_shelx_res_checksum              55186
_shelx_hkl_checksum              14870
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'