Isoreticular Series of (3,24)-Connected Metal‒Organic Frameworks: Facile Synthesis and High Methane Uptake Properties
Barin, Gokhan; Krungleviciute, Vaiva; Gomez-Gualdron, Diego A.; Sarjeant, Amy A.; Snurr, Randall Q.; Hupp, Joseph T.; Yildirim, Taner; Farha, Omar K.; Chemistry of Materials 26 (2014) 1912–; doi:10.1021/cm404155s

data_4001892
_publ_section_title
;
 Isoreticular Series of (3,24)-Connected Metal--Organic Frameworks: Facile
 Synthesis and High Methane Uptake Properties
;
_journal_issue                   5
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1912
_journal_paper_doi               10.1021/cm404155s
_journal_volume                  26
_journal_year                    2014
_chemical_formula_moiety         'C192 H96 Cu12 N40 O60'
_chemical_formula_sum            'C192 H96 Cu12 N40 O60'
_chemical_formula_weight         4685.56
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-04-10
_audit_creation_method
;
  Olex2 1.2
  (compiled Mar 21 2013 11:17:50, GUI svn.r4446)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.6853(6)
_cell_length_b                   34.6853(6)
_cell_length_c                   50.6917(13)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      57.99
_cell_measurement_theta_min      2.51
_cell_volume                     60986(2)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.769
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.769
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            84899
_diffrn_reflns_point_group_measured_fraction_full 0.769
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.77
_diffrn_reflns_theta_min         1.80
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.7515
_exptl_absorpt_correction_T_min  0.6370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0684 before and 0.0584 after correction.
The Ratio of minimum to maximum transmission is 0.8476.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.510
_exptl_crystal_description       block
_exptl_crystal_F_000             9424
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         21496
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1493P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2170
_refine_ls_wR_factor_ref         0.2337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10384
_reflns_number_total             21496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm404155s_si_003.cif
_cod_data_source_block           n2610_a
_cod_original_cell_volume        60986(3)
_cod_database_code               4001892
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N7-C41 \\sim N9-C42
 with sigma of 0.02
 N8-N7 \\sim N9-N8
 with sigma of 0.02
 N8-C41 \\sim N9-C41
 with sigma of 0.02
 C12-C11 \\sim C16-C11 \\sim C16-C15 \\sim C15-C14 \\sim C14-C13 \\sim C13-C12 
 \\sim C31-C30 \\sim C30-C29
 \\sim C29-C28 \\sim C28-C27 \\sim C32-C27 \\sim C32-C31 \\sim C46-C45 \\sim 
 C47-C46 \\sim C48-C47 \\sim C48-
 C43 \\sim C44-C43 \\sim C45-C44
 with sigma of 0.02
 C15-C13 \\sim C16-C12 \\sim C29-C31 \\sim C32-C28 \\sim C44-C48 \\sim C47-C45
 with sigma of 0.02
 C16-C13 \\sim C15-C12 \\sim C11-C14 \\sim C31-C28 \\sim C29-C32 \\sim C30-C27
 \\sim C45-C48 \\sim C44-C47
 \\sim C46-C43
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C9(H9), C12(H12), C13(H13), C15(H15), C16(H16),
 C19(H19), C21(H21), C23(H23), C25(H25), C28(H28), C29(H29), C31(H31), C32(H32),
  C35(H35), C37(H37), C39(H39), C48(H48), C47(H47), C45(H45), C44(H44), C41(H41)
;
_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 = 47479.0 Ang^3^ [77.9%]
Total electron count / cell = 10694.7
;
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.854
_shelxl_version_number           2012-9