Synthesis and characterization of low-nuclearity lantern-type porous coordination cages.
Taggart, Garrett A.; Lorzing, Gregory R.; Dworzak, Michael R.; Yap, Glenn P. A.; Bloch, Eric D.; Chemical communications (Cambridge, England) 56 (2020) 8924–8927; doi:10.1039/d0cc03266b

data_7126727
_publ_section_title
;
 Synthesis and characterization of low-nuclearity lantern-type porous
 coordination cages.
;
_journal_issue                   63
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8924
_journal_page_last               8927
_journal_paper_doi               10.1039/d0cc03266b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C90 H70 Cu4 N2 O19'
_chemical_formula_sum            'C90 H70 Cu4 N2 O19'
_chemical_formula_weight         1737.64
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-06-04
_audit_creation_method
; 
Olex2 1.2 
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2020-06-05 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8590(4)
_cell_length_b                   12.8590(4)
_cell_length_c                   23.9559(8)
_cell_measurement_reflns_used    4966
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      50.37
_cell_measurement_theta_min      3.69
_cell_volume                     3961.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10085
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        50.434
_diffrn_reflns_theta_max         50.434
_diffrn_reflns_theta_min         3.901
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Olex2 1.2 
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1074
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0739
_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^)+(0.1549P)^2^+19.7720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                893
_reflns_number_total             1074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03266b2.cif
_cod_data_source_block           eric411
_cod_depositor_comments
'Adding full bibliography for 7126725--7126728.cif.'
_cod_original_cell_volume        3961.2(3)
_cod_database_code               7126727
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Uiso/Uaniso restraints and constraints 
O4 \\sim C13 \\sim N1 \\sim C14 \\sim C15: within 2A with sigma of 0.002 and 
sigma for terminal atoms of 0.004 
3. Rigid body (RIGU) restrains 
 O4, C13, N1, C14, C15 
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 
4. Others 
 Fixed Sof: H12A(0.5) H12B(0.5) H12C(0.5) O4(0.25) C13(0.25) H13(0.25) 
 N1(0.25) C14(0.25) H14A(0.25) H14B(0.25) H14C(0.25) C15(0.25) H15A(0.25) 
 H15B(0.25) H15C(0.25) 
5.a Free rotating group: 
 O4(C13,N1,C14,C15) 
5.b Me refined with riding coordinates: 
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C) 
5.c Aromatic/amide H refined with riding coordinates: 
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C13(H13) 
5.d Idealised Me refined as rotating group: 
 C12(H12A,H12B,H12C) 
;
_shelx_res_checksum              2194
_olex2_submission_special_instructions 'No special instructions were received'