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_7034708
_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         'C60 H84 Cl4 Cu8 N8 O16, 4(C2 H5 O0.5)'
_chemical_formula_sum            'C68 H104 Cl4 Cu8 N8 O18'
_chemical_formula_weight         1971.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2014-10-16 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.74110(10)
_cell_length_b                   20.12890(10)
_cell_length_c                   51.7316(5)
_cell_measurement_reflns_used    77684
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      75.9440
_cell_measurement_theta_min      3.8530
_cell_volume                     16364.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -70.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   57.0000    0.0000 97

  2 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -180.0000 79

  3 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -150.0000 79

  4 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  -90.0000 79

  5 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000   90.0000 79

  6 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  120.0000 79

  7 omega -111.00  -16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  152.0000   63.9967 95

  8 omega   23.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000    0.0000 75

  9 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  150.0000 55

 10 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 82

 11 omega   99.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  115.0000  161.0000 79

 12 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 79

 13 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   30.0000 55

 14 omega   24.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000    0.0000 -180.0000 154

 15 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 82

 16 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 55

 17 omega   40.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 58

 18 omega   37.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000   90.0000 105

 19 omega   40.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  150.0000 58

 20 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -150.0000 55

 21 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   90.0000 55

 22 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 82

 23 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000    0.0000 84

 24 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 82

 25 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   90.0000 91

 26 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 79

 27 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 79

 28 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 82

 29 omega   80.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000  142.7898 98

 30 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 82

 31 omega   41.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -60.0000 98

 32 omega   31.00  156.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000 -180.0000 125

 33 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 55

 34 omega   40.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 58

 35 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 79

 36 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -123.0000  -27.4213 82

 37 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000   60.0000 96

 38 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000  -30.0000 96

 39 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  150.0000 105

 40 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000 -120.0000 96

 41 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000 -120.0000 105

 42 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000   60.0000 105

 43 omega   11.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686   81.0000  -86.8446 35

 44 omega   83.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -158.7046 95

 45 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000    0.0000 91

 46 omega   83.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 48

 47 omega   66.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -60.0000 112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0092388000
_diffrn_orient_matrix_UB_12      0.0060544000
_diffrn_orient_matrix_UB_13      0.0297170000
_diffrn_orient_matrix_UB_21      -0.0848032000
_diffrn_orient_matrix_UB_22      0.0382413000
_diffrn_orient_matrix_UB_23      -0.0002214000
_diffrn_orient_matrix_UB_31      -0.0482758000
_diffrn_orient_matrix_UB_32      -0.0660251000
_diffrn_orient_matrix_UB_33      0.0025985000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            200377
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.197
_diffrn_reflns_theta_min         3.378
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.997
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       block
_exptl_crystal_F_000             8096
_exptl_crystal_size_max          0.1101
_exptl_crystal_size_mid          0.0934
_exptl_crystal_size_min          0.0377
_refine_diff_density_max         1.913
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         17064
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0564P)^2^+128.6241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15363
_reflns_number_total             17064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00884k2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7034701--7034709.cif.'
_cod_database_code               7034708
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cu I'
_chemical_oxdiff_usercomment     '@ 200 K JF3243.1'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-H8 = O4-H4
 0.84 with sigma of 0.02
 O12-H12
 0.84 with sigma of 0.02
 O16-H16
 0.84 with sigma of 0.02
 C68-C67 \\sim C66-C65 \\sim C64-C63 \\sim C62-C61 \\sim C69-C70
 with sigma of 0.02
 O18-C67 \\sim O18-C66 \\sim O17-C63 \\sim O17-C62 \\sim O19-C69
 with sigma of 0.02
3. Rigid bond restraints
 C69, O19, C69, C70
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 C68, C67, O18, C66, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C70, C69, O19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C64, C63, O17, C62, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O17(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C62(0.5) H62A(0.5)
 H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
  C29(H29A,H29B), C30(H30A,H30B), C38(H38A,H38B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C53(H53A,H53B),
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B),
  C69(H69A,H69B), C62(H62A,H62B), C63(H63A,H63B), C66(H66A,H66B), C67(H67A,H67B)
6.b Me refined with riding coordinates:
 C25(H25A,H25B,H25C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C18(H18), C20(H20), C33(H33), C35(H35), C48(H48), C50(H50)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C70(H70A,
 H70B,H70C), C61(H61A,H61B,H61C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C68(H68A,H68B,H68C)
;
_shelx_res_checksum              7782
_olex2_exptl_crystal_mounting_method 'Mitegen tip, Paratone oil'
_olex2_submission_original_sample_id JF3243.1
_olex2_submission_special_instructions 'No special instructions were received'