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_7034707
_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         'C64 H88 Cu8 N8 O24, 5 C H4 O'
_chemical_formula_sum            'C69 H108 Cu8 N8 O29'
_chemical_formula_weight         2021.95
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           222
_space_group_name_Hall           '-P 4a 2bc 3'
_space_group_name_H-M_alt        'P n -3 n'
_symmetry_space_group_name_Hall  '-P 4a 2bc 3'
_symmetry_space_group_name_H-M   'P n -3 n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_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            24
_cell_length_a                   37.57080(16)
_cell_length_b                   37.57080(16)
_cell_length_c                   37.57080(16)
_cell_measurement_reflns_used    34890
_cell_measurement_temperature    120
_cell_measurement_theta_max      75.3000
_cell_measurement_theta_min      4.0510
_cell_volume                     53033.6(4)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120
_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 0.997
_diffrn_measurement_details
;
  1 omega  -50.00   28.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186   38.0000 -150.0000 104

  2 omega -116.00  -22.25   0.7500    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  -38.0000   60.0000 125

  3 omega   23.00   98.00   0.7500    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4186 -125.0000    0.0000 100

  4 omega   30.00  108.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 104

  5 omega   40.00   97.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 76

  6 omega   36.00   90.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -180.0000 72

  7 omega   83.00  154.25   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 95

  8 omega   99.00  176.25   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000 -120.0000 103

  9 omega   56.00  134.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  120.0000 104

 10 omega   53.00   79.25   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000    0.0000 35

 11 omega   89.00  119.00   0.7500   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 40
;
_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      0.0344990000
_diffrn_orient_matrix_UB_12      0.0057930000
_diffrn_orient_matrix_UB_13      -0.0214313000
_diffrn_orient_matrix_UB_21      -0.0022596000
_diffrn_orient_matrix_UB_22      -0.0384530000
_diffrn_orient_matrix_UB_23      -0.0139981000
_diffrn_orient_matrix_UB_31      -0.0221074000
_diffrn_orient_matrix_UB_32      0.0129503000
_diffrn_orient_matrix_UB_33      -0.0320103000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            232108
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.254
_diffrn_reflns_theta_min         3.327
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88551
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             25008
_exptl_crystal_recrystallization_method
'Diffusion of MeOH and MeCN solution into THF.'
_exptl_crystal_size_max          0.2369
_exptl_crystal_size_mid          0.1238
_exptl_crystal_size_min          0.0664
_platon_squeeze_details
' 5 molecules of solvent methanol per asymmetric unit'
_refine_diff_density_max         1.266
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         9253
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0707P)^2^+79.8921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7731
_reflns_number_total             9253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00884k2.cif
_cod_data_source_block           eb4124
_cod_depositor_comments
'Adding full bibliography for 7034701--7034709.cif.'
_cod_original_cell_volume        53033.6(7)
_cod_database_code               7034707
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C100 H200 Cu8 N20 O30 I'
_chemical_oxdiff_usercomment     '@ 120 K JF3144.2'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4 = O8-H8
 0.84 with sigma of 0.01
 C32-C31 \\sim C23-C18
 with sigma of 0.02
 O11-C31 \\sim O12-C31 \\sim O9-C29 \\sim O10-C29
 with sigma of 0.02
3. Rigid bond restraints
 C32, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C31 \\sim C32: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C31) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 O11, C31, O12, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9, C29, O10, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.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), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B)
6.b Me refined with riding coordinates:
 C32(H32A,H32B,H32C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              93566
_shelx_fab_checksum              89364
_olex2_exptl_crystal_mounting_method 'Mitegen tip, Paratone oil.'
_olex2_submission_original_sample_id JF3144.2
_olex2_submission_special_instructions 'No special instructions were received'