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_1512723
_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 Tm O15), Ca H12 O6, 3(H2 O)'
_chemical_formula_sum            'C24 H42 Ca3 O39 Tm2'
_chemical_formula_weight         1412.68
_chemical_name_systematic
;
Hexaaquacalcium bis(\m~3~-oxydiacetato)calciumthuliumate 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                   26.4117(9)
_cell_length_b                   26.4117(9)
_cell_length_c                   26.4117(9)
_cell_measurement_reflns_used    742
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.7176
_cell_measurement_theta_min      4.7317
_cell_volume                     18424.2(11)
_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      566(2)
_diffrn_detector_area_resol_mean 10.5953
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega -123.00  -97.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7531  -98.0000 -121.0000 26

  2 omega -119.00  -81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.7531 -125.0000 -180.0000 38

  3 omega   26.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      109.8081  -30.0000 -180.0000 64

  4 omega   35.00   70.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      109.8081  -37.0000  -96.0000 35
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0492888000
_diffrn_orient_matrix_UB_12      -0.0238485000
_diffrn_orient_matrix_UB_13      -0.0201415000
_diffrn_orient_matrix_UB_21      -0.0258724000
_diffrn_orient_matrix_UB_22      -0.0100374000
_diffrn_orient_matrix_UB_23      -0.0512683000
_diffrn_orient_matrix_UB_31      0.0175465000
_diffrn_orient_matrix_UB_32      0.0523249000
_diffrn_orient_matrix_UB_33      -0.0189943000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2946
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         71.78
_diffrn_reflns_theta_min         4.74
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.989
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             11136
_exptl_crystal_size_max          0.1056
_exptl_crystal_size_mid          0.0808
_exptl_crystal_size_min          0.0788
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0944P)^2^+50.5083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1626
_reflns_number_gt                576
_reflns_number_total             750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-196-202-7.cif
_cod_data_source_block           TmCaODA
_cod_original_cell_volume        18424.3(11)
_cod_database_code               1512723