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_4123500
_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         'C240 H126 N12 O32 Zr6'
_chemical_formula_sum            'C240 H126 N12 O32 Zr6'
_chemical_formula_weight         4236.84
_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             2014-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   28.9202(7)
_cell_length_b                   28.9202(7)
_cell_length_c                   28.9202(7)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.110
_cell_measurement_theta_min      2.647
_cell_volume                     24188.2(10)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.999
_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  0.0691
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48688
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.105
_diffrn_reflns_theta_min         1.527
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0717 before and 0.0549 after correction.
The Ratio of minimum to maximum transmission is 0.8488.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.291
_exptl_crystal_description       cube
_exptl_crystal_F_000             2146
_exptl_crystal_size_max          0.064
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         4009
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0672P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3316
_reflns_number_total             4009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja512973b_si_005.cif
_cod_data_source_block           n3463
_cod_depositor_comments
'Adding full bibliography for 4123497--4123500.cif.'
_cod_original_cell_volume        24188.2(18)
_cod_database_code               4123500
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.960
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C13-H13 = C12-H12
 0.95 with sigma of 0.0001
 C11-H12 = H13-C8
 2 with sigma of 0.0001
 H12-C13 = H13-C12
 2 with sigma of 0.0001
 C8-C13 \\sim C13-C12 \\sim C12-C11 \\sim C11-C10 \\sim C9-C10 \\sim C9-C8
 with sigma of 0.02
 C8-C11 \\sim C13-C10 \\sim C12-C9
 with sigma of 0.02
 C8-C12 \\sim C13-C11
 with sigma of 0.02
 C13-C11 \\sim C12-C10 \\sim C11-C9 \\sim C10-C8 \\sim C9-C13
 with sigma of 0.02
3. 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
4. Others
 Fixed Sof: N1(0.25) H1(0.125) C2(0.25) C3(0.5) H3(0.5) C4(0.5) H4(0.5)
 C5(0.25) C6(0.25) C7(0.25) C8(0.25) C9(0.25) H9(0.25) C10(0.25) H10(0.25)
 C11(0.25) H12(0.25) H13(0.25) C14(0.25) C15(0.5) C16(0.5) H16(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C9(H9), C10(H10), C16(H16)
;
_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 = 19042.1 Ang^3^ [78.7%]
Total electron count / cell = 736.1
;
_shelx_res_checksum              18456
_shelx_hkl_checksum              28350