Ascorbic acid decomposition into oxalate ions: a simple synthetic route towards oxalato-bridged heterometallic 3d-4f clusters.
Dinca, Alina S.; Shova, Sergiu; Ion, Adrian E.; Maxim, Catalin; Lloret, Francesc; Julve, Miguel; Andruh, Marius; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7148–7151; doi:10.1039/c5dt00778j

data_7034496
_publ_section_title
;
 Ascorbic acid decomposition into oxalate ions: a simple synthetic route
 towards oxalato-bridged heterometallic 3d-4f clusters.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7148
_journal_page_last               7151
_journal_paper_doi               10.1039/c5dt00778j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C138 H138 Cu6 Dy6 N12 O60, 5(H2 O)'
_chemical_formula_sum            'C138 H148 Cu6 Dy6 N12 O65'
_chemical_formula_weight         4370.92
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-19 deposited with the CCDC.
2015-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                116.101(3)
_cell_angle_beta                 100.935(3)
_cell_angle_gamma                92.943(2)
_cell_formula_units_Z            1
_cell_length_a                   15.0763(4)
_cell_length_b                   18.9062(6)
_cell_length_c                   19.3431(6)
_cell_measurement_reflns_used    7943
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      24.7780
_cell_measurement_theta_min      1.6080
_cell_volume                     4804.2(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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -76.00    1.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0914  -57.0000  -60.0000 77

  2 omega  -77.00   -9.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0914  -57.0000  150.0000 68

  3 omega  -80.00  -13.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0914  -57.0000   90.0000 67

  4 omega  -10.00   22.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0914  -99.0000    0.0000 32

  5 omega  -17.00   34.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0914   38.0000   60.0000 51

  6 omega  -39.00   52.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0914   77.0000 -120.0000 91
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0432830000
_diffrn_orient_matrix_UB_12      -0.0194324000
_diffrn_orient_matrix_UB_13      -0.0033826000
_diffrn_orient_matrix_UB_21      0.0068978000
_diffrn_orient_matrix_UB_22      -0.0348994000
_diffrn_orient_matrix_UB_23      -0.0321251000
_diffrn_orient_matrix_UB_31      0.0207373000
_diffrn_orient_matrix_UB_32      -0.0138388000
_diffrn_orient_matrix_UB_33      0.0268862000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.1367
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42447
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56702
_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            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2150
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.975
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         13698
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                9526
_reflns_number_total             13698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00778j2.cif
_cod_data_source_block           shi_2413_maan
_cod_depositor_comments
'Adding full bibliography for 7034494--7034500.cif.'
_cod_database_code               7034496
_chemical_oxdiff_formula         'C138 H144 Dy6 N12 Cu6 O63'
_chemical_oxdiff_usercomment     Cu6Dy6Asc_894
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H3WA,H3WB} of O3W, {H4WA,H4WB} of O4W, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H2WA,H2WB} of O2W, {H1WA,H1WB} of O1W
2. Restrained distances
 C69-C68 \\sim C69X-C68
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C69X) \\sim Ueq, Uanis(C69) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C69) = Uanis(C69X)
4. Others
 Fixed Sof: C69X(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C69(0.5) H69D(0.5)
 H69E(0.5) H69F(0.5) O3W(0.4) H3WA(0.4) H3WB(0.4) O4W(0.4) H4WA(0.4) H4WB(0.4)
 O2W(0.7) H2WA(0.7) H2WB(0.7)
5.a Riding coordinates:
 C69X(H69A,H69B,H69C), C69(H69D,H69E,H69F), O3W(H3WA,H3WB), O4W(H4WA,H4WB),
 O2W(H2WA,H2WB)
5.b Free rotating group:
 O1W(H1WA,H1WB)
5.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C14(H14), C15(H15), C16(H16),
 C28(H28), C29(H29), C30(H30), C33(H33), C37(H37), C39(H39), C40(H40), C41(H41),
  C47(H47), C48(H48), C49(H49), C52(H52), C56(H56), C58(H58), C59(H59), C60(H60)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C67(H67A,
 H67B,H67C)
;
_olex2_submission_special_instructions 'No special instructions were received'