Molecular Pac-Man and Tacos: layered Cu(ii) cages from ligands with high binding site concentrations.
McDonald, Cecelia; Williams, David W.; Comar, Priyanka; Coles, Simon J.; Keene, Tony D.; Pitak, Mateusz B.; Brechin, Euan K.; Jones, Leigh F.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13359–13368; doi:10.1039/c5dt01463h

data_7035558
_publ_section_title
;
 Molecular Pac-Man and Tacos: layered Cu(ii) cages from ligands with high
 binding site concentrations.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13359
_journal_page_last               13368
_journal_paper_doi               10.1039/c5dt01463h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C60.5 H55 Cu7 N8.5 O22.5, C62 H58 Cu7 N8 O21, 3(C H4 O), 3.5(N O3), 7(O)'
_chemical_formula_sum            'C125.5 H125 Cu14 N20 O64'
_chemical_formula_weight         3827.01
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Hygroscopic
_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
_audit_creation_date             2015-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-09 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                71.435(3)
_cell_angle_beta                 77.204(3)
_cell_angle_gamma                80.405(3)
_cell_formula_units_Z            2
_cell_length_a                   15.4185(6)
_cell_length_b                   22.8429(7)
_cell_length_c                   25.1092(9)
_cell_measurement_reflns_used    3877
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.5920
_cell_measurement_theta_min      3.1970
_cell_volume                     8130.8(5)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 '
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 '
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 '
_computing_molecular_graphics
;
Diamond 3.2k, 2014 Crystal Impact GbR (author: Klaus Brandenburg)
;
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.2782
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            69808
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.025
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 '
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH '
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.160
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2019
_refine_ls_number_reflns         28668
_refine_ls_number_restraints     4163
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1771
_refine_ls_R_factor_gt           0.0861
_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^)+(0.1027P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2038
_refine_ls_wR_factor_ref         0.2446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13027
_reflns_number_total             28668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01463h2.cif
_cod_data_source_block           compound2rev
_cod_depositor_comments
'Adding full bibliography for 7035553--7035558.cif.'
_cod_original_formula_sum        'C125.50 H125 Cu14 N20 O64'
_cod_database_code               7035558
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.834
_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, All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 N18-O51
 1.25 with sigma of 0.01
 N18-O50
 1.25 with sigma of 0.01
 N18-O52
 1.25 with sigma of 0.01
 N17-O47A
 1.25 with sigma of 0.02
 N17-O48A
 1.25 with sigma of 0.02
 N17-O49A
 1.25 with sigma of 0.02
 N19A-O53A
 1.25 with sigma of 0.02
 N19A-O54A
 1.25 with sigma of 0.02
 N19A-O55A
 1.25 with sigma of 0.02
 N19B-O53B
 1.25 with sigma of 0.02
 N19B-O54B
 1.25 with sigma of 0.02
 N19B-O55B
 1.25 with sigma of 0.02
 N20A-O60A
 1.25 with sigma of 0.01
 N20A-O61A
 1.25 with sigma of 0.01
 N20A-O62A
 1.25 with sigma of 0.01
 N20B-O60B
 1.25 with sigma of 0.01
 N20B-O61B
 1.25 with sigma of 0.01
 N20B-O62B
 1.25 with sigma of 0.01
 O62B-O60B
 2.6 with sigma of 0.01
 O53A-O66
 2.6 with sigma of 0.01
 O202-O207
 2.6 with sigma of 0.01
 O60C-C201
 1.44 with sigma of 0.01
 Cu6-O60B
 2.4 with sigma of 0.02
 Cu6-O60C
 2.5 with sigma of 0.02
 O43-H43
 0.87 with sigma of 0.01
 O40-H40A
 0.87 with sigma of 0.01
 O60C-H60D
 0.87 with sigma of 0.01
 O50-O51
 2.15 with sigma of 0.02
 O51-O52
 2.15 with sigma of 0.02
 O52-O50
 2.15 with sigma of 0.02
 O47A-O48A
 2.15 with sigma of 0.04
 O48A-O49A
 2.15 with sigma of 0.04
 O49A-O47A
 2.15 with sigma of 0.04
 O53A-O54A
 2.15 with sigma of 0.04
 O54A-O55A
 2.15 with sigma of 0.04
 O53A-O55A
 2.15 with sigma of 0.04
 O53B-O54B
 2.15 with sigma of 0.04
 O54B-O55B
 2.15 with sigma of 0.04
 O53B-O55B
 2.15 with sigma of 0.04
 O60A-O61A
 2.15 with sigma of 0.02
 O61A-O62A
 2.15 with sigma of 0.02
 O62A-O60A
 2.15 with sigma of 0.02
 O60B-O61B
 2.15 with sigma of 0.02
 O61B-O62B
 2.15 with sigma of 0.02
 O62B-O60B
 2.15 with sigma of 0.02
 O60B-O62B
 2.2 with sigma of 0.02
 O60B-O61B
 2.2 with sigma of 0.02
 O61B-O62B
 2.2 with sigma of 0.02
 Cu6-O60B
 3 with sigma of 0.04
 C124-H43
 1.892677 with sigma of 0.02
 Cu14-H43
 2.847984 with sigma of 0.02
 C123-H40A
 1.89737 with sigma of 0.02
 Cu11-H40A
 2.875858 with sigma of 0.02
 C201-H60D
 1.917726 with sigma of 0.02
 Cu6-H60D
 2.871517 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O60B) = Uanis(O62B) = Uanis(O61B)
Uiso(O60A) = Uiso(O61A) = Uiso(O62A)
Uanis(O60C) = Uanis(O60B)
Uanis(O47A) = Uanis(O47B)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O49B)=Sof(O47B)=Sof(O48B)=1-FVAR(1)
 Sof(O47A)=Sof(O48A)=Sof(O49A)=FVAR(1)
 Fixed Sof: N20A(0.5) O60A(0.5) O61A(0.5) O62A(0.5) O101(0.5) H10A(0.5)
 H10B(0.5) O203(0.5) O60C(0.5) C201(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 O60B(0.5) O62B(0.5) O61B(0.5) N20B(0.5) O200(0.5) O201(0.5) O202(0.5)
 O206(0.5) O204(0.5) O207(0.5) O208(0.5) N19B(0.5) O55B(0.5) O54B(0.5)
 O53B(0.5) N19A(0.5) O53A(0.5) O54A(0.5) O55A(0.5) H60D(0.5)
7.a Rotating group:
 O34(H34A,H34B), O35(H35A,H35B), O36(H36A,H36B), O37(H37A,H37B), O39(H39A,
 H39B), O41(H41A,H41B), O42(H42A,H42B), O101(H10A,H10B)
7.b Me refined with riding coordinates:
 C201(H20A,H20B,H20C)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12),
 C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C25(H25), C26(H26), C27(H27),
  C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C40(H40), C41(H41),
 C42(H42), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C55(H55), C56(H56),
  C57(H57), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C70(H70),
 C71(H71), C72(H72), C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C85(H85),
  C86(H86), C87(H87), C93(H93), C94(H94), C95(H95), C96(H96), C98(H98),
 C100(H100), C101(H101), C102(H102), C108(H108), C109(H109), C110(H110),
 C111(H111), C113(H113), C115(H115), C116(H116), C117(H117)
7.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C60(H60A,H60B,
 H60C), C75(H75A,H75B,H75C), C90(H90A,H90B,H90C), C105(H10C,H10D,H10E),
 C120(H12A,H12B,H12C), C123(H12D,H12E,H12F), C124(H12G,H12H,H12I), C125(H12J,
 H12K,H12L), C126(H12M,H12N,H12O), C127(H12P,H12Q,H12R)
7.e Idealised tetrahedral OH refined as rotating group:
 O44(H44), O45(H45), O46(H46)
;
_shelx_res_checksum              5919
_olex2_submission_special_instructions 'No special instructions were received'