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_7034499
_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
'C148 H165 Dy6 N12 Ni6 O66, C2 H3 N, 2.7(H2 O)'
_chemical_formula_sum            'C150 H173.4 Dy6 N13 Ni6 O68.7'
_chemical_formula_weight         4584.88
_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             2015-03-15
_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                90.00
_cell_angle_beta                 93.399(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1001(6)
_cell_length_b                   27.9469(9)
_cell_length_c                   25.5495(7)
_cell_measurement_reflns_used    7923
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      23.0310
_cell_measurement_theta_min      1.5560
_cell_volume                     10762.9(6)
_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      173.05(10)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -13.00   17.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0127  -99.0000   30.0000 30

  2 omega  -93.00  -45.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0127 -178.0000  -60.0000 48

  3 omega   -5.00   89.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5127   19.0000   60.0000 94

  4 omega  -11.00   39.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5127   77.0000 -150.0000 50

  5 omega  -22.00   37.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5127  -57.0000 -150.0000 59
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0145873000
_diffrn_orient_matrix_UB_12      0.0240924000
_diffrn_orient_matrix_UB_13      -0.0005460000
_diffrn_orient_matrix_UB_21      0.0447440000
_diffrn_orient_matrix_UB_22      -0.0078703000
_diffrn_orient_matrix_UB_23      0.0025093000
_diffrn_orient_matrix_UB_31      0.0009763000
_diffrn_orient_matrix_UB_32      -0.0012013000
_diffrn_orient_matrix_UB_33      -0.0276892000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1049
_diffrn_reflns_av_unetI/netI     0.2222
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62652
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.67
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.641
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61427
_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    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4556
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.750
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1101
_refine_ls_number_reflns         18236
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                9333
_reflns_number_total             18236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00778j2.cif
_cod_data_source_block           shi_2406_maan
_cod_depositor_comments
'Adding full bibliography for 7034494--7034500.cif.'
_cod_original_cell_volume        10763.0(6)
_cod_original_formula_sum        'C150 H173.40 Dy6 N13 Ni6 O68.70'
_cod_database_code               7034499
_chemical_oxdiff_formula         'C130 H140 Dy6 Ni6 N14 O70'
_chemical_oxdiff_usercomment     '_870 DyNi'
_reflns_odcompleteness_completeness 99.94
_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, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H1WA,H1WB} of O1W, {H4WA,H4WB} of O4W, {H2WA,H2WB} of
  O2W, {H31A,H31B} of O31
2. Restrained distances
 C76-C77
 1.5 with sigma of 0.1
 N7-C76
 1.18 with sigma of 0.1
 C72-C73 \\sim C75-C74 \\sim C75X-C74 \\sim C70-C71
 with sigma of 0.01
 O31-C70 \\sim O33-C74 \\sim O32-C72
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uiso(C75) = Uiso(C75X)
4. Others
 Fixed Sof: H31A(0.5) H31B(0.5) H74C(0.5) H74D(0.5) H74A(0.5) H74B(0.5)
 N7(0.5) O4W(0.25) H4WA(0.25) H4WB(0.25) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5)
 C75X(0.5) H75D(0.5) H75E(0.5) H75F(0.5) O2W(0.35) H2WA(0.35) H2WB(0.35)
 C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5) C76(0.5) O3W(0.25) H3WA(0.25)
 H3WB(0.25) O1W(0.5) H1WA(0.5) H1WB(0.5) C70(0.5) H70A(0.5) H70B(0.5) C71(0.5)
 H71A(0.5) H71B(0.5) H71C(0.5)
5.a Riding coordinates:
 O31(H31A,H31B), C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C67(H67A,H67B,H67C),
 C26(H26A,H26B,H26C), C69(H69A,H69B,H69C), C65(H65A,H65B,H65C), C73(H73A,H73B,
 H73C), O4W(H4WA,H4WB), C75(H75A,H75B,H75C), C75X(H75D,H75E,H75F), O2W(H2WA,
 H2WB), O3W(H3WA,H3WB), O1W(H1WA,H1WB), C71(H71A,H71B,H71C)
5.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C34(H34A,H34B), C55(H55A,H55B), C53(H53A,H53B), C54(H54A,
 H54B), C9(H9A,H9B), C74(H74C,H74D), C74(H74A,H74B), C35(H35A,H35B), C10(H10A,
 H10B), C11(H11A,H11B), C72(H72A,H72B), C70(H70A,H70B)
5.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C37(H37), C48(H48), C30(H30), C40(H40), C15(H15), C49(H49),
 C56(H56), C41(H41), C60(H60), C52(H52), C59(H59), C39(H39), C58(H58), C3(H3),
 C5(H5), C4(H4), C28(H28), C33(H33), C29(H29), C8(H8), C14(H14), C16(H16),
 C12(H12)
5.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C63(H63A,H63B,H63C), C45(H45A,H45B,H45C), C77(H77A,H77B,
 H77C)
;
_olex2_submission_special_instructions 'No special instructions were received'