Synthesis and Characterization of Tb[N(CN)2]3·2H2O and Eu[N(CN)2]3·2H2O: Two New Luminescent Rare-Earth Dicyanamides
Nag, Abanti; Schmidt, Peter J.; Schnick, Wolfgang; Chemistry of Materials 18 (2006) 5738–; doi:10.1021/cm0607029

data_4001561
_publ_section_title
;
 Synthesis and Characterization of Tb[N(CN)2]3&#x00B7;2H2O and
 Eu[N(CN)2]3&#x00B7;2H2O:&#x00A0; Two New Luminescent Rare-Earth
 Dicyanamides
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5738
_journal_paper_doi               10.1021/cm0607029
_journal_volume                  18
_journal_year                    2006
_chemical_formula_moiety         'C6 H4 N9 O2 Tb'
_chemical_formula_sum            'C6 H4 N9 O2 Tb'
_chemical_formula_weight         393.10
_chemical_name_common            'terbium dicyanamide dihydrate'
_chemical_name_systematic        'terbium dicyanamide dihydrate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4632(15)
_cell_length_b                   11.523(2)
_cell_length_c                   13.944(3)
_cell_measurement_reflns_used    177
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     1196.2(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo & Scalepack(Otwinowski & Minor 1997)'
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  'vertically 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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19462
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    5.923
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'ellipsoid correction based on equivalents'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2723
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.4464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0419
_reflns_number_gt                1992
_reflns_number_total             2723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm0607029si20060323_083638.cif
_cod_data_source_block           TbC6N9H4O2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4001561