Two new diamine templated lanthanum sulfates, La2(H2O)2(C4H12N2)(SO4)4 and La2(H2O)2(C2H10N2)3(SO4)6·4H2O, with 3D and 2D crystal structures
Thierry Bataille; Daniel Louër; J. Mater. Chem. 12 (2002) 3487–3493; doi:10.1039/b207212m

data_7204503
_publ_section_title
;
 Two new diamine templated lanthanum sulfates, La2(H2O)2(C4H12N2)(SO4)4
 and La2(H2O)2(C2H10N2)3(SO4)6&#x00B7;4H2O, with 3D and 2D crystal
 structures
;
_journal_issue                   12
_journal_name_full               'J. Mater. Chem.'
_journal_page_first              3487
_journal_page_last               3493
_journal_paper_doi               10.1039/b207212m
_journal_volume                  12
_journal_year                    2002
_chemical_formula_moiety         'La2 (H2 O)2 (C4 H12 N2) (S1 O4)4'
_chemical_formula_sum            'C4 H16 La2 N2 O18 S4'
_chemical_formula_weight         786.25
_chemical_name_common            'lanthanum piperazine sulfate dihydrate'
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 104.2164(4)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   16.7936(2)
_cell_length_b                   9.58580(10)
_cell_length_c                   22.5827(3)
_cell_measurement_reflns_used    12149
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.032
_cell_measurement_theta_min      0.998
_cell_volume                     3524.03(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al.,1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            53463
_diffrn_reflns_theta_full        32.04
_diffrn_reflns_theta_max         32.04
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    5.359
_exptl_absorpt_correction_T_max  0.81193
_exptl_absorpt_correction_T_min  0.40164
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'N.W. Alcock (1970). Cryst. Computing, p271)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.0375
_refine_diff_density_max         2.881
_refine_diff_density_min         -2.048
_refine_diff_density_rms         0.283
_refine_ls_extinction_coef       0.00021(5)
_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   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         12271
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                8634
_reflns_number_total             12271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207212m.txt
_cod_data_source_block           job
_cod_database_code               7204503