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_4132677
_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(C3 H7 N O)'
_chemical_formula_sum            'C46 H54 N2 O10'
_chemical_formula_weight         794.91
_chemical_name_common            MeMeCH2x2DMF
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                   15.482(3)
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_cell_length_c                   15.976(3)
_cell_measurement_reflns_used    3552
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.512
_cell_measurement_theta_min      2.214
_cell_volume                     4025.2(13)
_computing_cell_refinement       'SAINT V8.37A, Bruker-AXS'
_computing_data_collection       'APEX 2, Bruker-AXS'
_computing_data_reduction        'SAINT V8.37A, Bruker-AXS'
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_computing_structure_solution    'SHELXS-Version 2013/1, G. Sheldrick'
_diffrn_ambient_temperature      100(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  0.0372
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.815
_diffrn_source                   'sealed xray tube'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2, G. Sheldrick'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method DMF
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_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0135P)^2^+6.9572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3202
_reflns_number_total             3553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05471_si_003.cif
_cod_data_source_block           17010_MeMeCH2xDMF
_cod_original_cell_volume        4025.3(14)
_cod_database_code               4132677
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              95544
_shelx_hkl_checksum              83226