Ultrahigh Surface Area Zirconium MOFs and Insights into the Applicability of the BET Theory.
Wang, Timothy C.; Bury, Wojciech; Gómez-Gualdrón, Diego A; Vermeulen, Nicolaas A.; Mondloch, Joseph E.; Deria, Pravas; Zhang, Kainan; Moghadam, Peyman Z.; Sarjeant, Amy A.; Snurr, Randall Q.; Stoddart, J. Fraser; Hupp, Joseph T.; Farha, Omar K.; Journal of the American Chemical Society 137 (2015) 3585–3591; doi:10.1021/ja512973b

data_4123498
_publ_section_title
;
 Ultrahigh Surface Area Zirconium MOFs and Insights into the Applicability
 of the BET Theory.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3585
_journal_page_last               3591
_journal_paper_doi               10.1021/ja512973b
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C216 H120 N12 O32 Zr6'
_chemical_formula_sum            'C216 H120 N12 O32 Zr6'
_chemical_formula_weight         3942.55
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P m -3 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   25.3340(12)
_cell_length_b                   25.3340(12)
_cell_length_c                   25.3340(12)
_cell_measurement_reflns_used    9091
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      67.820
_cell_measurement_theta_min      2.466
_cell_volume                     16259.7(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            109260
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.119
_diffrn_reflns_theta_min         1.744
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.7334
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0690 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.9277.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.047
_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     84
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     305
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0564P)^2^+9.3944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2739
_reflns_number_total             2926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja512973b_si_003.cif
_cod_data_source_block           n3273
_cod_depositor_comments
'Adding full bibliography for 4123497--4123500.cif.'
_cod_original_cell_volume        16260(2)
_cod_database_code               4123498
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.884
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-H7
 0.94 with sigma of 0.001
 C3-C2 \\sim C4-C3 \\sim C5-C4 \\sim C7_$1-C6 \\sim C8_$1-C7_$1 \\sim C9-C8_$1
 with sigma of 0.02
 C2-C5 \\sim C3-C4_$1 \\sim C4-C3_$1 \\sim C6-C9 \\sim C7_$1-C8 \\sim C8_$1-C7
 with sigma of 0.02
 C3-C3_$1 \\sim C4-C4_$1 \\sim C7_$1-C7 \\sim C8_$1-C8 \\sim C2-C4 \\sim
C3_$1-C5 \\sim C6-C8_$1 \\sim C7-C9
 with sigma of 0.02
 C3_$1-C2 \\sim C3-C2 \\sim C4-C3 \\sim C5-C4 \\sim C5-C4_$1 \\sim C7_$1-C6
\\sim C7-C6 \\sim C8-C7 \\sim C9-
 C8 \\sim C9-C8_$1
 with sigma of 0.02
 C2-C5 \\sim C3-C4_$1 \\sim C3_$1-C4 \\sim C6-C9 \\sim C7_$1-C8 \\sim C7-C8_$1
 with sigma of 0.02
 C2-C4 \\sim C3-C5 \\sim C6-C8_$1 \\sim C7_$1-C9 \\sim C4-C4_$1 \\sim C5-C3_$1
\\sim C8_$1-C8 \\sim C9-C7
 \\sim C8-C6 \\sim C7-C7_$1 \\sim C4_$1-C2 \\sim C3_$1-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. 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
5. Others
 Fixed Sof: C7(0.5) H7(0.5) C8(0.5) H8(0.5)
6.a Riding coordinates and stretchable bonds:
 C7(H7)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C12(H12)
;
_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 = 13299.9 Ang^3^ [81.8%]
Total electron count / cell = 3478.1
;
_shelx_res_checksum              66453
_shelx_hkl_checksum              48193