Design and Synthesis of Capped-Paddlewheel-Based Porous Coordination Cages
Lorzing, Gregory; Gosselin, Eric; Lindner, Brian S.; Bhattacharjee, Rameswar; Yap, Glenn; Caratzoulas, Stavros; Bloch, Eric D.; Chemical Communications  (2019) –; doi:10.1039/C9CC05002G

data_7123866
_publ_section_title
;
 Design and Synthesis of Capped-Paddlewheel-Based Porous Coordination
 Cages
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05002G
_journal_year                    2019
_chemical_formula_moiety         'C180 H156 Cu12 N24 O59, 3 (Cl O4)'
_chemical_formula_sum            'C180 H156 Cl3 Cu12 N24 O71'
_chemical_formula_weight         4660.11
_chemical_name_systematic        '[Cu12(btc)4(OMe-bipy)12][ClO4]12'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-15 deposited with the CCDC.    2019-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                105.0947(11)
_cell_angle_beta                 92.9723(11)
_cell_angle_gamma                102.3211(14)
_cell_formula_units_Z            4
_cell_length_a                   22.8717(6)
_cell_length_b                   34.9204(9)
_cell_length_c                   36.9964(9)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.51
_cell_measurement_theta_min      2.54
_cell_volume                     27690.6(12)
_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      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0677
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            360091
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        53.159
_diffrn_reflns_theta_max         53.159
_diffrn_reflns_theta_min         1.245
_exptl_absorpt_coefficient_mu    1.826
_exptl_absorpt_correction_T_max  0.7504
_exptl_absorpt_correction_T_min  0.5978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             9484
_exptl_crystal_size_max          0.433
_exptl_crystal_size_mid          0.414
_exptl_crystal_size_min          0.216
_refine_diff_density_max         3.220
_refine_diff_density_min         -2.102
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.420
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4303
_refine_ls_number_reflns         62671
_refine_ls_number_restraints     9553
_refine_ls_restrained_S_all      2.418
_refine_ls_R_factor_all          0.2514
_refine_ls_R_factor_gt           0.2025
_refine_ls_shift/su_max          0.086
_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          0.5258
_refine_ls_wR_factor_ref         0.5821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                39759
_reflns_number_total             62671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05002g2.cif
_cod_data_source_block           eric212_sq
_cod_database_code               7123866
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.505
_shelx_estimated_absorpt_t_max   0.694
_shelx_res_checksum              27469
_shelx_fab_checksum              24677