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_7034495
_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 Gd6 N12 O60, 9(H2 O), 0.7(C3 H7 N1 O1)'
_chemical_formula_sum            'C140.1 H160.9 Cu6 Gd6 N12.7 O69.7'
_chemical_formula_weight         4462.66
_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                116.117(3)
_cell_angle_beta                 100.924(2)
_cell_angle_gamma                92.814(2)
_cell_formula_units_Z            1
_cell_length_a                   15.1096(4)
_cell_length_b                   18.9651(5)
_cell_length_c                   19.3767(6)
_cell_measurement_reflns_used    7468
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      26.2120
_cell_measurement_theta_min      1.9490
_cell_volume                     4839.6(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -22.00   20.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9352  -99.0000 -150.0000 42

  2 omega  -16.00   23.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9352  -99.0000  -30.0000 39

  3 omega  -25.00   52.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4352  -99.0000 -180.0000 77

  4 omega    4.00   41.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4352  -77.0000   60.0000 37

  5 omega  -41.00   85.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4352    0.0000  -30.0000 126

  6 omega  -43.00   31.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4352  -57.0000  -60.0000 74
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0389888000
_diffrn_orient_matrix_UB_12      -0.0235171000
_diffrn_orient_matrix_UB_13      -0.0302884000
_diffrn_orient_matrix_UB_21      -0.0103145000
_diffrn_orient_matrix_UB_22      -0.0181292000
_diffrn_orient_matrix_UB_23      0.0232470000
_diffrn_orient_matrix_UB_31      -0.0266856000
_diffrn_orient_matrix_UB_32      0.0298897000
_diffrn_orient_matrix_UB_33      0.0173718000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.1647
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45414
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83096
_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    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2206
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.694
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         16972
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                10753
_reflns_number_total             16972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00778j2.cif
_cod_data_source_block           shi_2414_maan
_cod_depositor_comments
'Adding full bibliography for 7034494--7034500.cif.'
_cod_original_cell_volume        4839.6(2)
_cod_original_formula_sum        'C140.10 H160.90 Cu6 Gd6 N12.70 O69.70'
_cod_database_code               7034495
_chemical_oxdiff_formula         'C138 H144 Gd6 N12 Cu6 O63'
_chemical_oxdiff_usercomment     'Cu6Gd6Asc .901'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2WA,H2WB} of O2W, {H7WA,H7WB} of O7W, {H8WA,H8WB} of O8W,
   {H1WA,H1WB} of O1W, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H6WA,H6WB} of O6W, {H10C,H10D} of O10W, {H9WA,H9WB}
  of O9W, {H5WA,H5WB} of O5W, {H3WA,H3WB} of O3W, {H4WA,H4WB} of O4W
2. Restrained distances
 N7-C71 = N7-C72
 1.47 with sigma of 0.01
 N7-C70
 1.4 with sigma of 0.01
 N7-C71 \\sim N7-C72
 with sigma of 0.01
 C72-C70 \\sim C70-C71
 with sigma of 0.001
3. Restrained planarity
 C70, C71, C72, N7, O31
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uiso(C71) = Uiso(N7) = Uiso(C72) = Uiso(C70) = Uiso(O31)
5. Others
 Fixed Sof: O10W(0.25) H10C(0.25) H10D(0.25) O6W(0.5) H6WA(0.5) H6WB(0.5)
 C70(0.35) H70(0.35) C71(0.35) H71A(0.35) H71B(0.35) H71C(0.35) C72(0.35)
 H72A(0.35) H72B(0.35) H72C(0.35) N7(0.35) O31(0.35) O7W(0.25) H7WA(0.25)
 H7WB(0.25) O2W(0.5) H2WA(0.5) H2WB(0.5) O9W(0.5) H9WA(0.5) H9WB(0.5) O4W(0.5)
 H4WA(0.5) H4WB(0.5) O3W(0.5) H3WA(0.5) H3WB(0.5) O5W(0.25) H5WA(0.25)
 H5WB(0.25) O8W(0.25) H8WA(0.25) H8WB(0.25)
6.a Riding coordinates:
 C65(H65A,H65B,H65C), C69(H69A,H69B,H69C), C67(H67A,H67B,H67C), O10W(H10C,
 H10D), O6W(H6WA,H6WB), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), O7W(H7WA,
 H7WB), O2W(H2WA,H2WB), O9W(H9WA,H9WB), O4W(H4WA,H4WB), O3W(H3WA,H3WB),
 O5W(H5WA,H5WB), O1W(H1WA,H1WB), O8W(H8WA,H8WB)
6.b 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)
6.c 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), C70(H70)
6.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)
;
_olex2_submission_special_instructions 'No special instructions were received'