Reinvestigation of layered poly[aquasodium(I) [[aquasamarium(III)]-di-μ-aqua-μ~3~-pyridine-2,6-dicarboxylato-μ~2~-pyridine-2,6-dicarboxylato] trihydrate]
Ikarashi, Kazuya; Taoyun, Zhu; Uematsu, Kazuyoshi; Toda, Kenji; Sato, Mineo; Acta Crystallographica Section E 63 (2007) m2203–m2204; doi:10.1107/S160053680702884X

data_2214926
_publ_section_title
;Reinvestigation of layered poly[aquasodium(I)
 [[aquasamarium(III)]-di-\m-aqua-\m~3~-pyridine-2,6-dicarboxylato-\m~2~-pyridine-2,6-dicarboxylato]
 trihydrate]
;
_journal_coeditor_code           YM2055
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2203
_journal_page_last               m2204
_journal_paper_doi               10.1107/S160053680702884X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Na Sm (C7 H3 N O4)2 (H2 O)4] , 3H2 O'
_chemical_formula_moiety         'C14 H14 N2 Na O12 Sm , 3H2 O'
_chemical_formula_sum            'C14 H20 N2 Na O15 Sm'
_chemical_formula_weight         629.66
_chemical_name_systematic
;
poly[aquasodium(I) [[aquasamarium(III)]-
di-\m-aqua-\m~3~-pyridine-2,6-dicarboxylato-\m~2~-pyridine-2,6-dicarboxylato]
trihydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.1630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2065(4)
_cell_length_b                   17.4485(3)
_cell_length_c                   11.3728(4)
_cell_measurement_reflns_used    19188
_cell_measurement_temperature    296
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.2
_cell_volume                     2201.27(12)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Rigaku R-AXIS-IV'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22103
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.9
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.968
_refine_diff_density_min         -1.278
_refine_ls_extinction_coef       0.00064(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6163
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0403P)^2^+2.6934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                5944
_reflns_number_total             6163
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ym2055.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2214926
_cod_database_fobs_code          2214926