Carborane-Based Metal‒Organic Framework with High Methane and Hydrogen Storage Capacities
Kennedy, Robert D.; Krungleviciute, Vaiva; Clingerman, Daniel J.; Mondloch, Joseph E.; Peng, Yang; Wilmer, Christopher E.; Sarjeant, Amy A.; Snurr, Randall Q.; Hupp, Joseph T.; Yildirim, Taner; Farha, Omar K.; Mirkin, Chad A.; Chemistry of Materials 25 (2013) 3539–; doi:10.1021/cm4020942

data_4001823
_publ_section_title
;
 Carborane-Based Metal--Organic Framework with High Methane and Hydrogen
 Storage Capacities
;
_journal_issue                   17
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3539
_journal_paper_doi               10.1021/cm4020942
_journal_volume                  25
_journal_year                    2013
_chemical_formula_moiety         'C9 H10 B5 Cu O5'
_chemical_formula_sum            'C9 H10 B5 Cu O5'
_chemical_formula_weight         315.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2012-08-14
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   18.6953(7)
_cell_length_b                   18.6953(7)
_cell_length_c                   39.1379(17)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.61
_cell_measurement_theta_min      2.96
_cell_volume                     11846.6(8)
_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
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_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  0.0576
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            25045
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        61.700
_diffrn_reflns_theta_max         61.72
_diffrn_reflns_theta_min         2.95
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  0.6295
_exptl_absorpt_correction_T_min  0.4596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1076 before and 0.0803 after correction.
The Ratio of minimum to maximum transmission is 0.7301.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.797
_exptl_crystal_description       prism
_exptl_crystal_F_000             2844
_exptl_crystal_recrystallization_method 'crystallized from DMF/H2O'
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.050
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.764
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2274
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.763
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.1173
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3735
_refine_ls_wR_factor_ref         0.3904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1873
_reflns_number_total             2274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm4020942_si_002.cif
_cod_data_source_block           NU-135
_cod_original_cell_volume        11846.6(10)
_cod_database_code               4001823
_diffrn_reflns_sigmai/neti       0.0271
_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.  Only the
atoms used in the refinement model are reported in the formula here.

Total solvent accessible volume / cell = 7491.7 Ang^3^ [63.2%]
Total electron count / cell = 1685.2
;
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.772
_shelx_hkl_checksum              8321
_shelx_res_checksum              41561
_shelxl_version_number           2012-4