Turning a "useless" ligand into a "useful" ligand: a magneto-structural study of an unusual family of Cu(II) wheels derived from functionalised phenolic oximes.
Frost, Jamie M.; Stirling, Robert J.; Sanz, Sergio; Vyas, Nidhi; Nichol, Gary S.; Rajaraman, Gopalan; Brechin, Euan K.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10177–10187; doi:10.1039/c5dt00884k

data_7034701
_publ_section_title
;
 Turning a &quot;useless&quot; ligand into a &quot;useful&quot; ligand: a
 magneto-structural study of an unusual family of Cu(II) wheels derived
 from functionalised phenolic oximes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10177
_journal_page_last               10187
_journal_paper_doi               10.1039/c5dt00884k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C56 H75 Cl4 Cu8 N8 O16 + solvent'
_chemical_formula_sum            'C56 H75 Cl4 Cu8 N8 O16'
_chemical_formula_weight         1766.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-27 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.5938(6)
_cell_length_b                   19.9423(4)
_cell_length_c                   32.2211(6)
_cell_measurement_reflns_used    12270
_cell_measurement_temperature    170
_cell_measurement_theta_max      25.7310
_cell_measurement_theta_min      3.3470
_cell_volume                     16445.6(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      170
_diffrn_detector                 Eos
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -86.00   42.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954   19.0000  -60.0000 256

  2 omega   -5.00   20.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  -99.0000 -150.0000 50

  3 omega   -8.00   25.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  -99.0000    0.0000 66

  4 omega  -70.00  -24.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  109.0000  171.4014 92

  5 omega   42.00  104.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2798  174.0000 -159.0000 124

  6 omega  -94.00    9.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  -57.0000  -90.0000 206

  7 omega  -98.00   20.00   0.5000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7954  -38.0000  120.0000 236
;
_diffrn_measurement_device       'Agilent Technologies XCalibur'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0262304000
_diffrn_orient_matrix_UB_12      0.0011572000
_diffrn_orient_matrix_UB_13      0.0070745000
_diffrn_orient_matrix_UB_21      0.0074861000
_diffrn_orient_matrix_UB_22      -0.0164999000
_diffrn_orient_matrix_UB_23      0.0185737000
_diffrn_orient_matrix_UB_31      0.0049025000
_diffrn_orient_matrix_UB_32      0.0314824000
_diffrn_orient_matrix_UB_33      0.0094693000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            97866
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        22.464
_diffrn_reflns_theta_max         22.464
_diffrn_reflns_theta_min         2.988
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  0.318
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             7160
_exptl_crystal_recrystallization_method
'Diffusion of ether, methanol and acetonitrile'
_exptl_crystal_size_max          0.4951
_exptl_crystal_size_mid          0.3405
_exptl_crystal_size_min          0.2465
_platon_squeeze_details          'see _refine_special_details'
_refine_diff_density_max         2.922
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         10680
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0529P)^2^+306.6443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8178
_reflns_number_total             10680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00884k2.cif
_cod_data_source_block           eb3251x1
_cod_depositor_comments
'Adding full bibliography for 7034701--7034709.cif.'
_cod_database_code               7034701
_chemical_oxdiff_formula         'C50 H50 N8 O20 Cu Cl'
_chemical_oxdiff_usercomment     '@ 120 K RS31/PS'
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     22.42
_platon_squeeze_void_probe_radius 1.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O16-H16
 0.87 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O4-H4
 0.87 with sigma of 0.01
 C56-H16
 1.916969 with sigma of 0.02
 Cu8-H16
 3.10123 with sigma of 0.02
 C42-H12
 1.927814 with sigma of 0.02
 Cu6-H12
 3.125451 with sigma of 0.02
 C14-H4
 1.903518 with sigma of 0.02
 Cu2-H4
 3.097624 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C27, C28, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C26(H26), C31(H31), C33(H33), C45(H45),
 C47(H47)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C)
5.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              50278
_shelx_fab_checksum              11879
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 5/11/13
_olex2_date_sample_submission    24/10/13
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Desktop Cooler'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'