Crystal structure and photoluminescence properties of lanthanide diphosphonates
Liu, Feng-Yi; Roces, Laura; Sa Ferreira, Rute A.; García-Granda, Santiago; García, José R.; Carlos, Luis D.; Rocha, João; Journal of Materials Chemistry 17 (2007) 3696–; doi:10.1039/b703487c

data_7202871
_publ_section_title
;
 Crystal structure and photoluminescence properties of lanthanide
 diphosphonates
;
_journal_issue                   35
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              3696
_journal_paper_doi               10.1039/b703487c
_journal_volume                  17
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C4 H11 La O14 P4, C4 H14 N2'
_chemical_formula_sum            'C8 H25 La N2 O14 P4'
_chemical_formula_weight         636.09
_chemical_name_common            (NH3(CH2)4NH3)La(hedpH)(hedpH2)
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-05-09T11:19:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                67.49(1)
_cell_angle_beta                 89.98(1)
_cell_angle_gamma                68.65(1)
_cell_formula_units_Z            2
_cell_length_a                   10.215(1)
_cell_length_b                   10.697(1)
_cell_length_c                   10.722(1)
_cell_measurement_reflns_used    2932
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.076
_cell_measurement_theta_min      2.209
_cell_measurement_wavelength     1.54184
_cell_volume                     994.8(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor )'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
Patterson methods using DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.104008
_diffrn_orient_matrix_UB_12      -0.57759E-1
_diffrn_orient_matrix_UB_13      0.355618E-1
_diffrn_orient_matrix_UB_21      -0.142265E-1
_diffrn_orient_matrix_UB_22      0.157321E-1
_diffrn_orient_matrix_UB_23      0.857973E-1
_diffrn_orient_matrix_UB_31      -0.174353E-1
_diffrn_orient_matrix_UB_32      -0.925025E-1
_diffrn_orient_matrix_UB_33      0.424591E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11560
_diffrn_reflns_theta_full        70
_diffrn_reflns_theta_max         70
_diffrn_reflns_theta_min         4.52
_diffrn_source                   'Nonius FR590'
_exptl_absorpt_coefficient_mu    20.339
_exptl_absorpt_correction_T_max  0.6658
_exptl_absorpt_correction_T_min  0.2234
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            colrless
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.48
_refine_diff_density_min         -1.48
_refine_diff_density_rms         0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3680
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1113P)^2^+2.7943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                3633
_reflns_number_total             3680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b703487c.txt
_cod_data_source_block           la01
_cod_database_code               7202871