Porous metal-organic alloys based on soluble coordination cages
Antonio, Alexandra M.; Korman, Kyle J.; Yap, Glenn; Bloch, Eric D.; Chemical Science  (2020) –; doi:10.1039/D0SC04941G

data_1559379
_publ_section_title
;
 Porous metal-organic alloys based on soluble coordination cages
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC04941G
_journal_year                    2020
_chemical_formula_moiety
; 
C264 H184 Cu24 N4 O144, 8[C6H13], 8[C5H11], 4[C4H9], 20[C3H7N] 
;
_chemical_formula_sum            'C428 H552 Cu24 N24 O144'
_chemical_formula_weight         9861.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-07-23 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.073(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   34.0993(15)
_cell_length_b                   34.2455(15)
_cell_length_c                   23.9647(11)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.42
_cell_measurement_theta_min      2.74
_cell_volume                     25746(2)
_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      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0753
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            84550
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        50.576
_diffrn_reflns_theta_max         50.576
_diffrn_reflns_theta_min         2.004
_exptl_absorpt_coefficient_mu    1.694
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 
RESPONSE: As in similar MOFs, this compound consistently deposits 
as weakly diffracting crystals. 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       Block
_exptl_crystal_F_000             10272
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.147
_refine_diff_density_max         1.472
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         13747
_refine_ls_number_restraints     1677
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0870
_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^)+(0.1658P)^2^+169.2353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2348
_refine_ls_wR_factor_ref         0.2950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8542
_reflns_number_total             13747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04941g2.cif
_cod_data_source_block           eric340
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               1559379
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.759
_shelx_estimated_absorpt_t_max   0.789
_shelx_res_checksum              42221
_shelx_fab_checksum              2052