Cation effect on the crystal structure of polynuclear complexes with 2,2'-oxydiacetate as bridging ligand
Julia Torres; Javier Gonzalez-Platas; Joaquin Sanchiz; Jorge Castiglioni; Sixto Dominguez; Carlos Kremer; Inorganica Chimica Acta 393 (2012) 196–202; doi:

data_1512720
_publ_section_title
;
 Cation effect on the crystal structure of polynuclear complexes with
 2,2'-oxydiacetate as bridging ligand
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              196
_journal_page_last               202
_journal_volume                  393
_journal_year                    2012
_chemical_formula_moiety         '2(C12 H12 Ca Ho O15), Ca H12 O6, 3(H2 O)'
_chemical_formula_sum            'C24 H42 Ca3 Ho2 O39'
_chemical_formula_weight         1404.68
_chemical_name_systematic
;
Hexaaquacalcium bis(\m~3~-oxydiacetato)calciumholmiumate trihydrate
;
_space_group_crystal_system      cubic
_space_group_IT_number           228
_space_group_name_H-M_alt        'F d -3 c'
_symmetry_space_group_name_Hall  '-F 4ud 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   26.4905(2)
_cell_length_b                   26.4905(2)
_cell_length_c                   26.4905(2)
_cell_measurement_reflns_used    3833
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.2090
_cell_measurement_theta_min      3.3339
_cell_volume                     18589.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
'Sir2011 (Burla et al., J. Appl. Cryst. 45, 2012)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5953
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega    5.00   40.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -120.0000 35

  2 omega   10.00   37.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -180.0000 27

  3 omega   14.00   39.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  150.0000 25

  4 omega -136.00  -82.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -54.9715 -109.0000  126.0000 54

  5 omega   94.00  141.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.9715  145.0000  109.0000 47

  6 omega  -34.00   -8.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.5000   38.0000  -30.0000 26

  7 omega -117.00  -61.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.5000 -145.0000   57.0000 56

  8 omega   67.00   93.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      109.9429  -38.0000 -120.0000 26

  9 omega   21.00   73.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      109.9429 -111.0000 -120.0000 52

 10 omega   51.00   89.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      109.9429  -25.0000 -180.0000 38

 11 omega  127.00  174.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      109.9429  109.0000 -137.0000 47

 12 omega   29.00   97.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      109.9429 -111.0000   60.0000 68

 13 omega   23.00   63.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      109.9429  -38.0000 -180.0000 40
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0068924000
_diffrn_orient_matrix_UB_12      0.0564008000
_diffrn_orient_matrix_UB_13      -0.0124971000
_diffrn_orient_matrix_UB_21      0.0576191000
_diffrn_orient_matrix_UB_22      0.0058222000
_diffrn_orient_matrix_UB_23      -0.0054427000
_diffrn_orient_matrix_UB_31      -0.0040025000
_diffrn_orient_matrix_UB_32      -0.0130060000
_diffrn_orient_matrix_UB_33      -0.0565043000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9107
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         71.35
_diffrn_reflns_theta_min         4.72
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.100
_exptl_absorpt_correction_T_max  0.157
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             11072
_exptl_crystal_size_max          0.3954
_exptl_crystal_size_mid          0.2938
_exptl_crystal_size_min          0.1836
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.000017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+119.3098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                689
_reflns_number_total             760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-196-202-4.cif
_cod_data_source_block           HoCaODA
_cod_database_code               1512720