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_7034704
_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 Cu8 N20 O16'
_chemical_formula_sum            'C67 H120 Cu8 N20 O27'
_chemical_formula_weight         2146.17
_chemical_name_systematic
;
 ?
;
_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     direct
_audit_creation_date             2013-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_audit_update_record
;
2014-10-16 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                   25.2990(5)
_cell_length_b                   20.7375(4)
_cell_length_c                   32.5445(8)
_cell_measurement_reflns_used    16475
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.8530
_cell_measurement_theta_min      3.8660
_cell_volume                     17074.1(6)
_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
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%$getVar(olex2_reference_short)%
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_computing_publication_material
;
%$getVar(olex2_reference_short)%
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_computing_structure_refinement
;
%$getVar(refinement_reference_short)%
;
_computing_structure_solution
;
%$getVar(solution_reference_short)%
;
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0085270000
_diffrn_orient_matrix_UB_12      0.0006366000
_diffrn_orient_matrix_UB_13      -0.0469074000
_diffrn_orient_matrix_UB_21      -0.0550907000
_diffrn_orient_matrix_UB_22      0.0301132000
_diffrn_orient_matrix_UB_23      0.0062288000
_diffrn_orient_matrix_UB_31      0.0244947000
_diffrn_orient_matrix_UB_32      0.0678523000
_diffrn_orient_matrix_UB_33      -0.0022842000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            87780
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.987
_diffrn_reflns_theta_min         3.072
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.883
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55452
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       plate
_exptl_crystal_F_000             8880
_exptl_crystal_size_max          0.4772
_exptl_crystal_size_mid          0.1391
_exptl_crystal_size_min          0.0295
_platon_squeeze_details
'11 MeOH per asymmetric unit removed with SQUEEZE'
_refine_diff_density_max         2.987
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         17342
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0956
_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^)+(0.1031P)^2^+162.7584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2426
_refine_ls_wR_factor_ref         0.2636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12269
_reflns_number_total             17342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00884k2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7034701--7034709.cif.'
_cod_database_code               7034704
_shelxl_version_number           2013-4
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C30 H40 N5 O10 Cu4'
_chemical_oxdiff_usercomment     '@ 120 K RS100(Et)'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
 O12-H12
 0.85 with sigma of 0.01
 O16-H16
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 C56-H12
 1.891964 with sigma of 0.02
 Cu6-H12
 3.078947 with sigma of 0.02
 C40-H16
 1.921845 with sigma of 0.02
 Cu8-H16
 3.121661 with sigma of 0.02
 C14-H4
 1.895716 with sigma of 0.02
 Cu2-H4
 3.135147 with sigma of 0.02
 C28-H8
 1.907963 with sigma of 0.02
 Cu4-H8
 3.07293 with sigma of 0.02
 Cu3-N12A \\sim Cu3-N12B \\sim Cu3-N12 \\sim Cu5-N15
 with sigma of 0.02
 N13A-N12A \\sim N13B-N12B \\sim N13-N12 \\sim N16-N15
 with sigma of 0.02
 N14A-N13A \\sim N14B-N13B \\sim N14-N13 \\sim N17-N16
 with sigma of 0.02
 N12A-N14A \\sim N15-N17
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N12, N13, N14, Cu3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 1*[Sof(N12)+Sof(N13)+Sof(N14)]+1*[Sof(N12B)+Sof(N13B)+Sof(N14B)]+1*[Sof(N12A)+
 Sof(N13A)+Sof(N14A)]=1 with esd of 0.001
 Sof(N12)=Sof(N13)=Sof(N14)=FVAR(1)
 Sof(N12B)=Sof(N13B)=Sof(N14B)=FVAR(2)
 Sof(N12A)=Sof(N13A)=Sof(N14A)=FVAR(3)
 Fixed Uiso: N12A(0.05) N12B(0.05) N13A(0.05) N13B(0.05) N14A(0.05) N14B(0.05)
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), C26(H26A,H26B), 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), 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)
;
_shelx_res_checksum              78155
_shelx_fab_checksum              11115