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_7034706
_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 H78 Cu4 N8 Na2 O16, 2.5 C H4 O'
_chemical_formula_sum            'C58.5 H84 Cu4 N8 Na2 O18.5'
_chemical_formula_weight         1495.47
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-27 deposited with the CCDC.
2015-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.295(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2213(3)
_cell_length_b                   26.3669(6)
_cell_length_c                   17.2409(4)
_cell_measurement_reflns_used    11836
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.1480
_cell_measurement_theta_min      3.0920
_cell_volume                     6908.0(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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
  1 omega  -76.00    9.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -57.0000  150.0000 85

  2 omega  -70.00  -43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -19.0000  -90.0000 27

  3 omega  -15.00   16.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -19.0000  -90.0000 31

  4 omega  -81.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -77.0000   60.0000 81

  5 omega  -67.00  -35.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  132.0000 -116.5641 32

  6 omega  -28.00   27.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352   38.0000  150.0000 55

  7 omega  -42.00    1.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352   19.0000   30.0000 43

  8 omega   36.00   63.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352   19.0000   30.0000 27

  9 omega  -38.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -77.0000  -90.0000 38

 10 omega   24.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633 -125.0000  -52.0766 27

 11 omega  -19.00   36.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -99.0000  -30.0000 55

 12 omega  -42.00  -15.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -38.0000    0.0000 27

 13 omega  -30.00   46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352   38.0000   90.0000 76
;
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0088758000
_diffrn_orient_matrix_UB_12      0.0263376000
_diffrn_orient_matrix_UB_13      0.0025292000
_diffrn_orient_matrix_UB_21      -0.0347079000
_diffrn_orient_matrix_UB_22      -0.0051507000
_diffrn_orient_matrix_UB_23      0.0246082000
_diffrn_orient_matrix_UB_31      0.0299335000
_diffrn_orient_matrix_UB_32      0.0018291000
_diffrn_orient_matrix_UB_33      0.0329514000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57914
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.887
_diffrn_reflns_theta_min         2.826
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.948
_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            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             3108
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of methanol and diethyl ether by solvent layering'
_exptl_crystal_size_max          0.2457
_exptl_crystal_size_mid          0.1298
_exptl_crystal_size_min          0.0164
_platon_squeeze_details          '2.5 methanol per asymmetric unit'
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         8317
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0384P)^2^+14.6993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5909
_reflns_number_total             8317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00884k2.cif
_cod_data_source_block           eb3275b
_cod_depositor_comments
'Adding full bibliography for 7034701--7034709.cif.'
_cod_original_formula_sum        'C58.50 H84 Cu4 N8 Na2 O18.50'
_cod_database_code               7034706
_chemical_oxdiff_formula         'C30 H50 N10 O20 Cu8 B F4'
_chemical_oxdiff_usercomment     '@ 120 K RS60'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_platon_squeeze_void_probe_radius 1.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H3 of O3, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H7 of O7, H8 of O8
2. Restrained distances
 O3-H3
 0.84 with sigma of 0.01
3.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)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C17(H17), C19(H19)
3.c Tetrahedral OH refined with riding coordinates:
 O7(H7), O8(H8)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              2035
_shelx_fab_checksum              7101
_shelx_shelxl_version_number     2014/7
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_date_sample_data_collection 18/11/13
_olex2_date_sample_submission    13/11/13
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'