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_7034705
_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 H76 Cu6 N8 O16'
_chemical_formula_sum            'C56 H76 Cu6 N8 O16'
_chemical_formula_weight         1498.48
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2015-03-27 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.153(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5984(3)
_cell_length_b                   26.6204(7)
_cell_length_c                   18.8428(4)
_cell_measurement_reflns_used    11838
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      74.6490
_cell_measurement_theta_min      3.7910
_cell_volume                     7100.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_temperature      120.0
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0927246000
_diffrn_orient_matrix_UB_12      0.0239937000
_diffrn_orient_matrix_UB_13      -0.0085632000
_diffrn_orient_matrix_UB_21      -0.0480045000
_diffrn_orient_matrix_UB_22      0.0519058000
_diffrn_orient_matrix_UB_23      -0.0101383000
_diffrn_orient_matrix_UB_31      0.0306523000
_diffrn_orient_matrix_UB_32      0.0088225000
_diffrn_orient_matrix_UB_33      0.0833000000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44755
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.802
_diffrn_reflns_theta_min         3.320
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.487
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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    1.402
_exptl_crystal_description       needle
_exptl_crystal_F_000             3080
_exptl_crystal_recrystallization_method
'Diffusion of hexane into a methanol solution'
_exptl_crystal_size_max          0.2685
_exptl_crystal_size_mid          0.0398
_exptl_crystal_size_min          0.0303
_platon_squeeze_details          '2.6 molecules of hexane per asymmetric unit'
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7393
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+11.4089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5830
_reflns_number_total             7393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00884k2.cif
_cod_data_source_block           eb4022
_cod_depositor_comments
'Adding full bibliography for 7034701--7034709.cif.'
_cod_database_code               7034705
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cu'
_chemical_oxdiff_usercomment     '@ 120 K JF2966.2'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H8' of O8', H4 of O4, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8
2. Restrained distances
 C28'-C27' \\sim C28-C27
 with sigma of 0.02
 O8-C28 \\sim O8'-C28' \\sim O4-C14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28') \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.1
Uanis(O8') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C28, O8, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27', C28', O8'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O8')=Sof(H8')=Sof(C27')=Sof(H27C)=Sof(H27D)=Sof(C28')=Sof(H28C)=Sof(H28D)=
 1-FVAR(1)
 Sof(O8)=Sof(H8)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 FVAR(1)
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),
 C27'(H27C,H27D), C28(H28A,H28B), C28'(H28C,H28D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19)
6.c Tetrahedral OH refined with riding coordinates:
 O8'(H8')
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
6.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O8(H8)
;
_shelx_res_checksum              34115
_shelx_fab_checksum              95110