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_7034703
_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
'C80 H98 Cu8 N12 O20, 2.78(C H4 O), 2(B F4), 2(C4 H10 O1)'
_chemical_formula_sum            'C90.78 H129.13 B2 Cu8 F8 N12 O24.78'
_chemical_formula_weight         2467.01
_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     direct
_audit_creation_date             2013-11-15
_audit_creation_method
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Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2014-10-16 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.0240(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3511(4)
_cell_length_b                   17.1783(2)
_cell_length_c                   26.2510(5)
_cell_measurement_reflns_used    24681
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      30.9620
_cell_measurement_theta_min      3.5540
_cell_volume                     10335.8(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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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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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Olex2
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_computing_publication_material
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Olex2
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_computing_structure_refinement
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ShelXL
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_computing_structure_solution
;
XT
;
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9105
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0273581000
_diffrn_orient_matrix_UB_12      0.0027017000
_diffrn_orient_matrix_UB_13      -0.0171667000
_diffrn_orient_matrix_UB_21      0.0029172000
_diffrn_orient_matrix_UB_22      0.0410660000
_diffrn_orient_matrix_UB_23      -0.0005555000
_diffrn_orient_matrix_UB_31      0.0141689000
_diffrn_orient_matrix_UB_32      -0.0032020000
_diffrn_orient_matrix_UB_33      -0.0215221000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            72031
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.211
_diffrn_reflns_theta_min         2.850
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       block
_exptl_crystal_F_000             5080
_exptl_crystal_size_max          0.4570
_exptl_crystal_size_mid          0.2853
_exptl_crystal_size_min          0.2033
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         15269
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0407P)^2^+28.5670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12230
_reflns_number_total             15269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00884k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7034701--7034709.cif.'
_cod_database_code               7034703
_shelxl_version_number           2013-4
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cu8 B F4'
_chemical_oxdiff_usercomment     '@ 120 K RS34'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H12 of O12, H3 of O3, H8 of O8, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H13 of O13
2. Restrained distances
 C42A-C43A
 2.5 with sigma of 0.04
 C41-C42 \\sim C43-C44
 with sigma of 0.02
 O11-C42 \\sim O11-C43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C41, C42, O11, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C41, C42, O11, C43, C44}
as
{C41A, C42A, O11A, C43A, C44A}
6. Others
 Sof(O13)=Sof(H13)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
 Sof(B1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(2)
 Sof(B1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(2)
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42C)=Sof(H42D)=
 Sof(O11A)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=1-FVAR(3)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(O11)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(3)
7.a Everything fixed:
 C41A, C42A, O11A, C43A, C44A
7.b 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), C42(H42A,H42B), C43(H43A,H43B), C42A(H42C,H42D), C43A(H43C,
 H43D)
7.c Me refined with riding coordinates:
 C41A(H41D,H41E,H41F), C44A(H44D,H44E,H44F)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C17(H17), C19(H19), C29(H29), C30(H30), C31(H31), C32(H32),
 C35(H35), C36(H36), C37(H37), C38(H38)
7.e Tetrahedral OH refined with riding coordinates:
 O13(H13)
7.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C40(H40A,H40B,H40C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C41(H41A,H41B,
 H41C), C44(H44A,H44B,H44C)
7.g Idealised tetrahedral OH refined as rotating group:
 O3(H3), O8(H8), O12(H12)
;
_shelx_res_checksum              91768