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_7034497
_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 Eu6 N12 O60 Zn6'
_chemical_formula_sum            'C141 H165.6 Eu6 N13 O71.3 Zn6'
_chemical_formula_weight         4487.25
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-16
_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                90.00
_cell_angle_beta                 91.157(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.3521(11)
_cell_length_b                   26.8468(17)
_cell_length_c                   24.981(2)
_cell_measurement_reflns_used    3494
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      18.4030
_cell_measurement_theta_min      1.5300
_cell_volume                     10293.9(13)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -23.00   25.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1690  -99.0000  -30.0000 48

  2 omega  -53.00   34.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690  -38.0000   30.0000 87

  3 omega  -49.00  -13.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690  -57.0000  150.0000 36

  4 omega   12.00   38.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690  -57.0000  150.0000 26

  5 omega   -6.00   23.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690  102.0000  174.0838 29
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0339840000
_diffrn_orient_matrix_UB_12      0.0178737000
_diffrn_orient_matrix_UB_13      0.0005802000
_diffrn_orient_matrix_UB_21      0.0090451000
_diffrn_orient_matrix_UB_22      -0.0054102000
_diffrn_orient_matrix_UB_23      -0.0271291000
_diffrn_orient_matrix_UB_31      -0.0299813000
_diffrn_orient_matrix_UB_32      0.0186929000
_diffrn_orient_matrix_UB_33      -0.0083673000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1549
_diffrn_reflns_av_unetI/netI     0.3470
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            47068
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66048
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4462
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.035
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         20931
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.2110
_refine_ls_R_factor_gt           0.0864
_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^)+(0.0083P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                6731
_reflns_number_total             20931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00778j2.cif
_cod_data_source_block           shi_2428_maan
_cod_depositor_comments
'Adding full bibliography for 7034494--7034500.cif.'
_cod_original_cell_volume        10293.7(13)
_cod_original_formula_sum        'C141 H165.60 Eu6 N13 O71.30 Zn6'
_cod_database_code               7034497
_chemical_oxdiff_formula         'C100 H40 N4 O30 Zn6 Eu6'
_chemical_oxdiff_usercomment     Zn_Eu
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Restrained distances
 H8-H9A
 2 with sigma of 0.01
 O25-C64 \\sim O26-C64 \\sim O29-C68 \\sim O30-C68 \\sim O28-C66 \\sim O27-C66
 with sigma of 0.01
 C67-C66 \\sim C69-C68 \\sim C65-C64
 with sigma of 0.01
 C11-C10 \\sim C9-C10
 with sigma of 0.01
 N2-C11 \\sim N1-C9
 with sigma of 0.01
 C13-C12 \\sim C8-C6
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C8 \\sim C9 \\sim C10 \\sim C11 \\sim N1: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C20) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a 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)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C14(H14), C15(H15), C16(H16),
 C30(H30), C29(H29), C28(H28), C33(H33), C37(H37), C41(H41), C40(H40), C39(H39),
  C47(H47), C48(H48), C49(H49), C52(H52), C56(H56), C58(H58), C59(H59), C60(H60)
4.c Fitted hexagon refined as free rotating group:
 C6(C7,C2,C3,C4,C5), C14(C15,C16,C17,C18,C13), C30(C29,C28,C27,C32,C31),
 C38(C43,C42,C41,C40,C39), C51(C46,C47,C48,C49,C50), C62(C57,C58,C59,C60,C61)
4.d 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), C69(H69A,H69B,H69C)
;
_olex2_submission_special_instructions 'No special instructions were received'