The key role of accurate lattice parameters in revealing subtle structural differences—a case study in the system [Ln(phen/phen-d8)2(NO3)3]
Werner, Franz; Tada, Kentaro; Ishii, Ayumi; Takata, Masaki; Hasegawa, Miki; CrystEngComm 11 (2009) 1197–; doi:10.1039/b904694c

data_7201079
_publ_section_title
;
 The key role of accurate lattice parameters in revealing subtle
 structural differences---a case study in the system
 [Ln(phen/phen-d8)2(NO3)3]
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1197
_journal_paper_doi               10.1039/b904694c
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'Eu 3+, (C12 H8 N2)2, (N O3 1-)3'
_chemical_formula_sum            'C24 H16 Eu N7 O9'
_chemical_formula_weight         698.39
_chemical_name_systematic
;
Tris(nitrato-O,O')bis(1,10-phenanthroline-N,N')europium(III)"
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2008-12-30
_cell_angle_alpha                90.0
_cell_angle_beta                 93.4580(6)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   9.52609(8)
_cell_length_b                   15.46723(16)
_cell_length_c                   17.22783(16)
_cell_measurement_temperature    300
_cell_volume                     2533.77(4)
_computing_structure_refinement  'GSAS (A.C. Larson, R.B. Von Dreele, 2004)'
_diffrn_ambient_temperature      300
_diffrn_detector                 'imaging plate'
_diffrn_radiation_monochromator  'Si 1 1 1 double-crystal monochromator'
_diffrn_radiation_polarisn_ratio 1.0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.00224
_diffrn_source                   synchrotron
_diffrn_source_type              'SPring-8, Beamline BL02B2'
_exptl_absorpt_correction_T_max  0.19395
_exptl_absorpt_correction_T_min  0.16872
_exptl_absorpt_process_details
; GSAS Absorption/surface roughness correction: function number 0
Debye-Scherrer absorption correction
Term (= MU.r/wave) = 1.0962
Correction is not refined.
;
_exptl_crystal_density_diffrn    1.831
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  colourless
_pd_instr_location
;
Large Debye-Scherrer camera, SPring-8, Japan
;
_pd_meas_scan_method             fixed
_pd_phase_name                   '[Eu(phen)2(NO3)3], modification IIa'
_pd_proc_ls_background_function
; GSAS Background function number 1 with 11 terms.
Shifted Chebyshev function of 1st kind
1: 987.394 2: -137.196 3: -54.2889 4: 61.6319
5: -35.5009 6: -31.2578 7: 33.7686 8: -8.09754
9: -12.3103 10: 24.7847 11: -18.8897
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_profile_function
;
CW Profile function number 4 with 21 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
Microstrain broadening by P.W. Stephens, (1999). J. Appl. Cryst.,32,281-289.
;
_pd_proc_ls_prof_R_factor        0.0264
_pd_proc_ls_prof_wR_expected     0.0252
_pd_proc_ls_prof_wR_factor       0.0337
_pd_spec_mounting                'Mark tube (diameter 0.3 mm)'
_pd_spec_mount_mode              transmission
_pd_spec_preparation             'gently ground'
_pd_spec_shape                   cylinder
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.35
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     115
_refine_ls_number_restraints     91
_refine_ls_R_Fsqd_factor         0.05144
_refine_ls_shift/su_max          0.08
_refine_ls_shift/su_mean         0.00
_refine_ls_weighting_scheme      sigma
_reflns_d_resolution_high        1.023
_reflns_d_resolution_low         8.598
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_total             1243
_cod_data_source_file            b904694c.txt
_cod_data_source_block           EUPHEN_2
_cod_original_cell_volume        2533.77(5)
_cod_database_code               7201079