Methane Storage in Paddlewheel-Based Porous Coordination Cages.
Rowland, Casey A.; Lorzing, Gregory R.; Gosselin, Eric J.; Trump, Benjamin A.; Yap, Glenn P. A.; Brown, Craig M.; Bloch, Eric D.; Journal of the American Chemical Society 140 (2018) 11153–11157; doi:10.1021/jacs.8b05780

data_4132718
_publ_section_title
;
 Methane Storage in Paddlewheel-Based Porous Coordination Cages.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11153
_journal_page_last               11157
_journal_paper_doi               10.1021/jacs.8b05780
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C168 H84 Mo12 N12 O68'
_chemical_formula_sum            'C168 H84 Mo12 N12 O68'
_chemical_formula_weight         4509.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 97.1210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.1875(5)
_cell_length_b                   28.6009(7)
_cell_length_c                   24.5462(5)
_cell_measurement_reflns_used    9101
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      56.34
_cell_measurement_theta_min      2.38
_cell_volume                     16849.7(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            159454
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.337
_diffrn_reflns_theta_min         2.383
_exptl_absorpt_coefficient_mu    3.954
_exptl_absorpt_correction_T_max  0.7511
_exptl_absorpt_correction_T_min  0.4918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX3 (Bruker, 2015)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.889
_exptl_crystal_description       block
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.557
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.195
_refine_diff_density_max         2.114
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         32201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1383P)^2^+119.8751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2286
_refine_ls_wR_factor_ref         0.2929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20898
_reflns_number_total             32201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05780_si_004.cif
_cod_data_source_block           eric128_sq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132718
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.217
_shelx_estimated_absorpt_t_max   0.513
_shelx_res_checksum              87945
_shelx_hkl_checksum              7632
_shelx_fab_checksum              11251