Two isomorphous lanthanide crotonate complexes: di-μ-but-2-enoato-bis[diaquabis(but-2-enoato)dysprosium(III)] adenine monosolvate heptahydrate and the samarium(II) analogue
Atria, Ana María; Garland, Maria Teresa; Baggio, Ricardo; Acta Crystallographica Section C 68 (2012) m80–m84; doi:10.1107/S0108270112007263

data_2018427
_publ_section_title
;
 Two isomorphous lanthanide crotonate complexes:
 di-\m-but-2-enoato-bis[diaquabis(but-2-enoato)dysprosium(III)] adenine
 monosolvate heptahydrate and the samarium(II) analogue
;
_journal_coeditor_code           SK3428
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m80
_journal_page_last               m84
_journal_paper_doi               10.1107/S0108270112007263
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Sm (C4 H5 O2)6 (H2 O)4] , C5 H5 N5 , 7H2 O'
_chemical_formula_moiety         'C24 H38 Sm2 O16, C5 H5 N5, 7(H2 O)'
_chemical_formula_sum            'C29 H57 N5 O23 Sm2'
_chemical_formula_weight         1144.50
_chemical_name_systematic
;
di-\m-but-2-enoato-bis[diaquabis(but-2-enoato)samarium(III)]
adenine monosolvate heptahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL97
_cell_angle_alpha                73.126(4)
_cell_angle_beta                 83.926(4)
_cell_angle_gamma                61.784(5)
_cell_formula_units_Z            1
_cell_length_a                   10.633(3)
_cell_length_b                   10.847(3)
_cell_length_c                   11.397(3)
_cell_measurement_reflns_used    9182
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.87
_cell_volume                     1107.6(5)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8609
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.710
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-NT; Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.503
_refine_ls_extinction_coef       0.0148(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4295
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0170
_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^)+(0.0221P)^2^+0.3677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                4154
_reflns_number_total             4295
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3428.cif
_cod_data_source_block           II
_cod_original_cell_volume        1107.7(5)
_cod_database_code               2018427
_cod_database_fobs_code          2018427