Use of a "Shoe-Last" Solid-State Template in the Mechanochemical Synthesis of High-Porosity RHO-Zinc Imidazolate.
Brekalo, Ivana; Kane, Christopher M.; Ley, Amanda N.; Ramirez, Joseph R.; Friščić, Tomislav; Holman, K. Travis; Journal of the American Chemical Society 140 (2018) 10104–10108; doi:10.1021/jacs.8b05471

data_4132678
_publ_section_title
;
 Use of a &quot;Shoe-Last&quot; Solid-State Template in the
 Mechanochemical Synthesis of High-Porosity RHO-Zinc Imidazolate.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10104
_journal_page_last               10108
_journal_paper_doi               10.1021/jacs.8b05471
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'8(C12 H12 N8 Zn2),C40 H40 O8,24(C3 H7 N1 O1)'
_chemical_formula_sum            'C208 H304 N88 O32 Zn16'
_chemical_formula_weight         5595.29
_chemical_name_common            MeMeCH2@rhoZnIm2-xDMF
_chemical_name_systematic        xMeMeCH2@rhoZn16Im32-xDMF
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            3
_cell_length_a                   28.6715(14)
_cell_length_b                   28.6715(14)
_cell_length_c                   28.6715(14)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.25
_cell_volume                     23570(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'X-SEED, L.Barbour (1999); http://x-seed.net/'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELX-2013-1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX DUO/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            198908
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         1.230
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker, 2014)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       'cubic block'
_exptl_crystal_F_000             8712
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.328
_exptl_crystal_size_min          0.187
_refine_diff_density_max         2.855
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         4033
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      2.073
_refine_ls_R_factor_all          0.1851
_refine_ls_R_factor_gt           0.1227
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_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          0.4312
_refine_ls_wR_factor_ref         0.5047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2405
_reflns_number_total             4033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05471_si_001.cif
_cod_data_source_block           16113_MeMeCH2@rhoZnIm2_sq
_cod_original_cell_volume        23570(3)
_cod_database_code               4132678
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.682
_shelx_estimated_absorpt_t_max   0.798
_shelx_res_checksum              97519
_shelx_hkl_checksum              86756
_shelx_fab_checksum              39323