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_7035554
_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         '2(C61.5 H50 Br4 Cu7 N8 O20.8), 0.5(O2)'
_chemical_formula_sum            'C123 H101.17 Br8 Cu14 N16 O42.58'
_chemical_formula_weight         4013.52
_chemical_name_common            '[Cu14]'
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-05
_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                90
_cell_angle_beta                 94.2850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   47.208(3)
_cell_length_b                   16.6283(12)
_cell_length_c                   21.3697(15)
_cell_measurement_reflns_used    47404
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     16728(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2014)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2014)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2014)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL2013 (Sheldrick, 2013)'
_computing_structure_solution    'ShelXS2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56525
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         1.978
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    3.723
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DTABSCOR
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             7911
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH '
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.478
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         19105
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+0.6691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12747
_reflns_number_total             19105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01463h2.cif
_cod_data_source_block           c2c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035553--7035558.cif.
;
_cod_database_code               7035554
_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
2. Restrained distances
 O99-H99
 0.85 with sigma of 0.01
 O104-H104
 0.85 with sigma of 0.01
 C100-H99
 1.967116 with sigma of 0.02
 Cu6-H99
 2.902776 with sigma of 0.02
 C105-H104
 1.88249 with sigma of 0.02
 Cu2-H104
 2.832376 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O104 \\sim O103 \\sim C105: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O73B \\sim O73A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Others
 Fixed Sof: Cu5B(0.5) C87B(0.5) H87B(0.5) C90B(0.5) H90B(0.5) C89B(0.5)
 H89B(0.5) O93B(0.5) C92B(0.5) C91B(0.5) Cu5A(0.5) O73A(0.5) O98(0.5) C92A(0.5)
 O93A(0.5) C86B(0.5) O104(0.5) H104(0.5) O96(0.5) C91A(0.5) C90A(0.5) H90A(0.5)
 C89A(0.5) H89A(0.5) C88A(0.5) H88A(0.5) C87A(0.5) H87A(0.5) C86A(0.5)
 O73B(0.5) C88B(0.5) H88B(0.5) O103(0.5) C105(0.5) H10H(0.5) H10I(0.5) H10J(0.5)
5.a Rotating group:
 O101(H10D,H10E), O102(H10F,H10G)
5.b Aromatic/amide H refined with riding coordinates:
 C87B(H87B), C90B(H90B), C89B(H89B), C37(H37), C62(H62), C19(H19), C84(H84),
 C55(H55), C67(H67), C58(H58), C44(H44), C17(H17), C41(H41), C68(H68), C22(H22),
  C77(H77), C80(H80), C23(H23), C34(H34), C25(H25), C14(H14), C47(H47),
 C46(H46), C66(H66), C65(H65), C90A(H90A), C89A(H89A), C88A(H88A), C87A(H87A),
 C45(H45), C24(H24), C88B(H88B)
5.c Fitted hexagon refined as free rotating group:
 C91A(C90A,C89A,C88A,C87A,C86A)
5.d Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C100(H10A,H10B,H10C), C11(H11A,H11B,H11C), C31(H31A,H31B,
 H31C), C52(H52A,H52B,H52C), C105(H10H,H10I,H10J)
;
_shelx_res_checksum              21284
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'