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_7034500
_publ_section_title
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 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 Dy6 N12 O60 Zn6, 5.5(C H4 O), 6.1(H2 O)'
_chemical_formula_sum            'C143.5 H172.2 Dy6 N12 O71.6 Zn6'
_chemical_formula_weight         4577.95
_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             2015-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.858(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1130(3)
_cell_length_b                   26.5550(4)
_cell_length_c                   24.6138(5)
_cell_measurement_temperature    293(2)
_cell_volume                     9877.0(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3442
_diffrn_reflns_av_unetI/netI     0.3780
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            72738
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.20
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.035
_exptl_absorpt_correction_T_max  0.7933
_exptl_absorpt_correction_T_min  0.5820
_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    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4532
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.661
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         14116
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.661
_refine_ls_R_factor_all          0.2338
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1662
_reflns_number_gt                3465
_reflns_number_total             14116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00778j2.cif
_cod_data_source_block           zndyasc
_cod_depositor_comments
'Adding full bibliography for 7034494--7034500.cif.'
_cod_original_formula_sum        'C143.50 H172.20 Dy6 N12 O71.60 Zn6'
_cod_database_code               7034500
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5WA,H5WB} of O5W, {H6WA,H6WB} of O6W, {H1WA,H1WB} of O1W,
   All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H2WA,H2WB} of O2W, {H4WA,H4WB} of O4W, {H3WA,H3WB} of
  O3W, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C34 \\sim N3: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O33(0.5) H33A(0.5) O31(0.75) H31(0.75) O32(0.5) H32(0.5) O4W(0.75)
 H4WA(0.75) H4WB(0.75) O1W(0.5) H1WA(0.5) H1WB(0.5) O6W(0.4) H6WA(0.4)
 H6WB(0.4) O5W(0.4) H5WA(0.4) H5WB(0.4) C8AA(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5)
 O2W(0.5) H2WA(0.5) H2WB(0.5) C70(0.75) H70A(0.75) H70B(0.75) H70C(0.75)
 C71(0.5) H71A(0.5) H71B(0.5) H71C(0.5) O3W(0.5) H3WA(0.5) H3WB(0.5)
4.a Riding coordinates:
 C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C1(H1A,H1B,H1C), C44(H44A,H44B,
 H44C), C39(H39), C26(H26A,H26B,H26C), C69(H69A,H69B,H69C), O31(H31), O32(H32),
 O4W(H4WA,H4WB), C72(H72A,H72B,H72C), O1W(H1WA,H1WB), O6W(H6WA,H6WB), O5W(H5WA,
 H5WB), C8AA(H8AA,H8AB,H8AC), O2W(H2WA,H2WB), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), O3W(H3WA,H3WB)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C9(H9A,H9B), C55(H55A,H55B), C54(H54A,H54B),
 C53(H53A,H53B), C36(H36A,H36B), C35(H35A,H35B), C34(H34A,H34B)
4.c Me refined with riding coordinates:
 C67(H67A,H67B,H67C), C45(H45A,H45B,H45C), C19(H19A,H19B,H19C)
4.d Aromatic/amide H refined with riding coordinates:
 C60(H60), C59(H59), C58(H58), C3(H3), C4(H4), C5(H5), C8(H8), C56(H56),
 C52(H52), C49(H49), C47(H47), C48(H48), C37(H37), C41(H41), C40(H40), C33(H33),
  C29(H29), C30(H30), C28(H28), C15(H15), C14(H14), C16(H16), C12(H12)
4.e Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C2)
4.f Tetrahedral OH refined with riding coordinates:
 O33(H33A)
4.g Idealised tetrahedral OH refined as rotating group:
 O34(H34)
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_olex2_submission_special_instructions 'No special instructions were received'