Redetermination at 180K of a layered lanthanide‒organic framework
Silva, Patrícia; Fernandes, José A.; Almeida Paz, Filipe A.; Acta Crystallographica Section E 68 (2012) m294–m295; doi:10.1107/S1600536812005508

data_2233815
_publ_section_title
;
 Redetermination at 180K of a layered lanthanide--organic framework
;
_journal_coeditor_code           GK2450
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m294
_journal_page_last               m295
_journal_paper_doi               10.1107/S1600536812005508
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[La (C3 H9 N O9 P3)]'
_chemical_formula_moiety         'C3 H9 La N O9 P3'
_chemical_formula_sum            'C3 H9 La N O9 P3'
_chemical_formula_weight         434.93
_chemical_name_common
;
poly[[\m~4~-nitrilotris(methylenephosphonic acid)(3-)]lanthanum(III)]
;
_chemical_name_systematic
;
poly[(\m~4~-{[bis(hydrogen
phosphonatomethyl)azaniumyl]methyl}phosphonato)lanthanum(III)]
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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            4
_cell_length_a                   9.144(3)
_cell_length_b                   11.727(4)
_cell_length_c                   9.823(3)
_cell_measurement_reflns_used    3599
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.94
_cell_measurement_theta_min      3.47
_cell_volume                     1053.3(6)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8 KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_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  0.1065
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31245
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    4.550
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.005
_refine_diff_density_max         3.982
_refine_diff_density_min         -1.632
_refine_ls_abs_structure_details 'Flack (1983), Friedel pairs 1229'
_refine_ls_abs_structure_Flack   0.44(4)
_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2728
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                1980
_reflns_number_total             2728
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2450.cif
_cod_data_source_block           I
_cod_database_code               2233815
_cod_database_fobs_code          2233815