Mechanochemical Synthesis of Porous Molecular Assemblies
Barreda, Omar; Taggart, Garrett A.; Rowland, Casey A.; Yap, Glenn P. A.; Bloch, Eric D.; Chemistry of Materials 30 (2018) 3975–; doi:10.1021/acs.chemmater.8b01667

data_4003365
_publ_section_title
;
 Mechanochemical Synthesis of Porous Molecular Assemblies
;
_journal_issue                   12
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3975
_journal_paper_doi               10.1021/acs.chemmater.8b01667
_journal_volume                  30
_journal_year                    2018
_chemical_formula_sum            'C276 H180 Cu24 N24 O144'
_chemical_formula_weight         7661.39
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.5662(17)
_cell_length_b                   32.5662(17)
_cell_length_c                   46.870(2)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      40.14
_cell_measurement_theta_min      3.18
_cell_volume                     49708(4)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            54059
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        40.409
_diffrn_reflns_theta_max         40.409
_diffrn_reflns_theta_min         1.652
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.5083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX3 (Bruker, 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.512
_exptl_crystal_description       block
_exptl_crystal_F_000             7704
_exptl_crystal_size_max          0.559
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.257
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         7734
_refine_ls_number_restraints     1090
_refine_ls_restrained_S_all      1.921
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.1325
_refine_ls_shift/su_max          0.005
_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          0.3954
_refine_ls_wR_factor_ref         0.4118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6664
_reflns_number_total             7734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b01667_si_002.cif
_cod_data_source_block           eric185_sq
_cod_original_cell_volume        49708(6)
_cod_database_code               4003365
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.657
_shelx_estimated_absorpt_t_max   0.817
_shelx_res_checksum              58766
_shelx_hkl_checksum              15610
_shelx_fab_checksum              41637