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_4132676
_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         'C40 H40 O8, 2(C5 H11 N O)'
_chemical_formula_sum            'C50 H62 N2 O10'
_chemical_formula_weight         850.9
_chemical_name_common            MeMeCH2x2DEF
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.143(8)
_cell_length_b                   15.393(5)
_cell_length_c                   12.944(5)
_cell_measurement_reflns_used    1091
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.339
_cell_measurement_theta_min      2.202
_cell_volume                     4611(3)
_computing_cell_refinement       'SAINT V8.37A, Bruker-AXS'
_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_data_reduction        'SAINT V8.37A, Bruker-AXS'
_computing_molecular_graphics    'X-SEED, L. Barbour (1999)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-Version 2013/1, G. Sheldrick'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            43854
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.760
_diffrn_source                   'sealed xray tube'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2, G. Sheldrick'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_recrystallization_method DEF
_exptl_crystal_size_max          0.361
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1692P)^2^+2.2844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2140
_refine_ls_wR_factor_ref         0.2370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3224
_reflns_number_total             4228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05471_si_002.cif
_cod_data_source_block           17045_MeMeCH2xDEF
_cod_database_code               4132676
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              40124
_shelx_hkl_checksum              95233