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_7034702
_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_absolute_configuration ad
_chemical_formula_moiety         'C56 H76 Cl0.79 Cu8 N11.21 O25.62'
_chemical_formula_sum            'C56 H76 Cl0.79 Cu8 N11.21 O25.62'
_chemical_formula_weight         1852.53
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           171
_space_group_name_Hall           'P 62'
_space_group_name_H-M_alt        'P 62'
_symmetry_space_group_name_Hall  'P 62'
_symmetry_space_group_name_H-M   'P 62'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_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                120
_cell_formula_units_Z            3
_cell_length_a                   20.2162(4)
_cell_length_b                   20.2162(4)
_cell_length_c                   16.8492(3)
_cell_measurement_reflns_used    13218
_cell_measurement_temperature    170
_cell_measurement_theta_max      22.2360
_cell_measurement_theta_min      3.4920
_cell_volume                     5963.6(2)
_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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Olex2
;
_computing_publication_material
;
Olex2
;
_computing_structure_refinement
;
ShelXL
;
_computing_structure_solution
;
Superflip
;
_diffrn_ambient_temperature      170
_diffrn_detector                 Eos
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9963
_diffrn_measured_fraction_theta_max 0.9967
_diffrn_measurement_device       'Agilent Technologies XCalibur'
_diffrn_measurement_device_type  'Agilent Technologies XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0113346000
_diffrn_orient_matrix_UB_12      0.0389124000
_diffrn_orient_matrix_UB_13      -0.0065287000
_diffrn_orient_matrix_UB_21      -0.0381831000
_diffrn_orient_matrix_UB_22      -0.0085014000
_diffrn_orient_matrix_UB_23      0.0060941000
_diffrn_orient_matrix_UB_31      0.0074484000
_diffrn_orient_matrix_UB_32      0.0074311000
_diffrn_orient_matrix_UB_33      0.0411292000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.720
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            74631
_diffrn_reflns_point_group_measured_fraction_full 0.718
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.460
_diffrn_reflns_theta_min         3.078
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80574
_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    1.547
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2823
_exptl_crystal_recrystallization_method
'From diffusion of diethyl ether, methanol and acetonitrile.'
_exptl_crystal_size_length       0.000
_exptl_crystal_size_max          0.6545
_exptl_crystal_size_mid          0.1271
_exptl_crystal_size_min          0.084
_exptl_crystal_size_rad          0.000
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 2144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.010(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         5175
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+2.0020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.715
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4751
_reflns_number_total             5175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00884k2.cif
_cod_data_source_block           eb3252
_cod_depositor_comments
'Adding full bibliography for 7034701--7034709.cif.'
_cod_original_cell_volume        5963.6(3)
_cod_database_code               7034702
_shelxl_version_number           2013-4
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C40 H80 N10 O20 Cu2'
_chemical_oxdiff_usercomment     '@ 170 K RS30/PS'
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     22.42
_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. Rigid bond restraints
 Cu2, O15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(Cl1')=1-FVAR(1)
 Sof(O13)=Sof(O14)=Sof(O15)=Sof(N6)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C00W(H00A,H00B), 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)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C17(H17), C19(H19)
4.c Tetrahedral OH refined with riding coordinates:
 O3(H3), O7(H7)
4.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              47049