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_7034498
_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         'C29 H28 Gd N2 Ni2 O17, 12(H2 O)'
_chemical_formula_sum            'C29 H52 Gd N2 Ni2 O29'
_chemical_formula_weight         1167.40
_chemical_name_systematic
;
 ? 
;
_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   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
;
2015-02-15 deposited with the CCDC.
2015-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.935(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.7331(11)
_cell_length_b                   17.0913(6)
_cell_length_c                   25.6958(14)
_cell_measurement_reflns_used    3531
_cell_measurement_temperature    199.8(4)
_cell_measurement_theta_max      29.1753
_cell_measurement_theta_min      2.3731
_cell_volume                     9734.9(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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      199.8(4)
_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  -90.00  -64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0127 -178.0000  150.0000 26

  2 omega  -16.00   10.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0127  -99.0000    0.0000 26

  3 omega   64.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690  178.0000   60.0000 28

  4 omega  -53.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690    0.0000  -60.0000 144

  5 omega   -6.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690   38.0000  120.0000 25

  6 omega  -53.00   45.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690  -38.0000  120.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0171655000
_diffrn_orient_matrix_UB_12      -0.0341322000
_diffrn_orient_matrix_UB_13      0.0004430000
_diffrn_orient_matrix_UB_21      0.0028375000
_diffrn_orient_matrix_UB_22      0.0115532000
_diffrn_orient_matrix_UB_23      -0.0254662000
_diffrn_orient_matrix_UB_31      0.0268557000
_diffrn_orient_matrix_UB_32      0.0205885000
_diffrn_orient_matrix_UB_33      0.0149957000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_unetI/netI     0.1193
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            24557
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.38
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         6948
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0732
_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^)+(0.0819P)^2^+41.0974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1929
_reflns_number_gt                4484
_reflns_number_total             6948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00778j2.cif
_cod_data_source_block           exp_1692
_cod_depositor_comments
'Adding full bibliography for 7034494--7034500.cif.'
_cod_original_cell_volume        9734.9(8)
_cod_database_code               7034498
_chemical_oxdiff_formula         'C16 H20 N2 O8 Ni1 Cd1'
_chemical_oxdiff_usercomment     '115/7, galben, 0.4x0.2x0.15'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O1V(0.25) H1VA(0.25) H1VB(0.25) O27W(0.2) H27A(0.2) H27B(0.2)
 O12W(0.8) H12A(0.8) H12B(0.8) O10W(0.5) H10A(0.5) H10B(0.5) O24W(0.55)
 H24A(0.55) H24B(0.55) O16W(0.45) H16A(0.45) H16B(0.45) O6W(0.3) H6WA(0.3)
 H6WB(0.3) O17W(0.5) H17A(0.5) H17B(0.5) O21W(0.5) H21A(0.5) H21B(0.5)
 O20W(0.75) H20A(0.75) H20B(0.75) O19W(0.5) H19A(0.5) H19B(0.5) O23W(0.5)
 H23A(0.5) H23B(0.5) O26W(0.4) H26D(0.4) H26E(0.4) O28W(0.5) H28A(0.5)
 H28B(0.5) O5W(0.2) H5WA(0.2) H5WB(0.2) O22W(0.4) H22A(0.4) H22B(0.4) O9W(0.2)
 H9WA(0.2) H9WB(0.2) O13W(0.25) H13D(0.25) H13E(0.25) O18W(0.5) H18A(0.5)
 H18B(0.5) O7W(0.35) H7WA(0.35) H7WB(0.35) O25W(0.5) H25A(0.5) H25B(0.5)
 O8W(0.4) H8WA(0.4) H8WB(0.4) O15W(0.4) H15A(0.4) H15B(0.4) O11W(0.75)
 H11A(0.75) H11B(0.75) O14W(0.35) H14D(0.35) H14E(0.35)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O4W(H4WA,H4WB), C1(H1A,H1B,H1C), C3(H3),
 C6(H6), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16), C19(H19), C26(H26A,
 H26B,H26C), O1V(H1VA,H1VB), O27W(H27A,H27B), O3W(H3WA,H3WB), O12W(H12A,H12B),
 O10W(H10A,H10B), O24W(H24A,H24B), O16W(H16A,H16B), O6W(H6WA,H6WB), O17W(H17A,
 H17B), O21W(H21A,H21B), O20W(H20A,H20B), O19W(H19A,H19B), O23W(H23A,H23B),
 O26W(H26D,H26E), O28W(H28A,H28B), O5W(H5WA,H5WB), O22W(H22A,H22B), O9W(H9WA,
 H9WB), O13W(H13D,H13E), O18W(H18A,H18B), O7W(H7WA,H7WB), O25W(H25A,H25B),
 O8W(H8WA,H8WB), O15W(H15A,H15B), O11W(H11A,H11B), O14W(H14D,H14E)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C11(H11), C20(H20), C21(H21), C24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'