#------------------------------------------------------------------------------
#$Date: 2016-03-21 00:21:50 +0100 (lun 21 de mar de 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/15/4001561.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4001561
loop_
_publ_author_name
'Nag, Abanti'
'Schmidt, Peter J.'
'Schnick, Wolfgang'
_publ_section_title
;
 Synthesis and Characterization of Tb[N(CN)2]3·2H2O and
 Eu[N(CN)2]3·2H2O:  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/[σ²(Fo²)+(0.0000P)²+0.4464P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Tb1 Tb 0.055977(17) 0.251066(14) 0.430837(8) 0.0316(3) Uani 1 1 d .
C2 C 0.1884(4) 0.3615(3) 0.0453(2) 0.0380(8) Uani 1 1 d .
N5 N 0.5496(5) 0.1265(4) 0.2621(2) 0.0704(12) Uani 1 1 d .
N4 N 0.3556(4) 0.2019(3) 0.3804(2) 0.0452(7) Uani 1 1 d .
N2 N 0.0538(4) 0.3827(3) 0.09783(19) 0.0523(9) Uani 1 1 d .
C4 C 0.5295(5) 0.1478(3) 0.1710(2) 0.0436(8) Uani 1 1 d .
N1 N 0.0570(5) 0.3167(4) 0.2642(2) 0.0634(10) Uani 1 1 d .
C1 C 0.0628(5) 0.3460(3) 0.1864(2) 0.0469(9) Uani 1 1 d .
C3 C 0.4425(4) 0.1686(3) 0.3218(2) 0.0405(8) Uani 1 1 d .
O1 O 0.2280(4) 0.4252(2) 0.4417(2) 0.0522(7) Uani 1 1 d D
H1 H 0.309(5) 0.437(3) 0.402(3) 0.078 Uiso 1 1 d D
H2 H 0.199(5) 0.493(2) 0.463(3) 0.078 Uiso 1 1 d D
N6 N 0.0251(4) 0.3417(3) 0.5893(2) 0.0520(8) Uani 1 1 d .
N7 N 0.0045(4) 0.0736(3) 0.3320(2) 0.0531(8) Uani 1 1 d .
N3 N -0.1984(4) 0.1520(3) 0.4951(2) 0.0447(7) Uani 1 1 d .
O2 O 0.1827(3) 0.1136(2) 0.54257(18) 0.0454(6) Uani 1 1 d D
H3 H 0.297(2) 0.107(3) 0.552(3) 0.068 Uiso 1 1 d D
H4 H 0.137(4) 0.051(2) 0.561(3) 0.068 Uiso 1 1 d D
N9 N -0.2039(4) 0.3807(3) 0.3960(2) 0.0501(8) Uani 1 1 d .
C6 C -0.3262(5) 0.4223(3) 0.3567(2) 0.0421(8) Uani 1 1 d .
N8 N -0.4770(4) 0.4677(3) 0.3203(2) 0.0562(9) Uani 1 1 d .
C5 C -0.0169(4) 0.0238(3) 0.2607(3) 0.0438(8) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Tb1 O1 109.45(10) . .
O2 Tb1 N3 74.38(9) . .
O1 Tb1 N3 143.22(9) . .
O2 Tb1 N1 143.47(10) . .
O1 Tb1 N1 76.23(12) . .
N3 Tb1 N1 123.27(11) . .
O2 Tb1 N4 72.86(9) . .
O1 Tb1 N4 73.46(10) . .
N3 Tb1 N4 138.15(10) . .
N1 Tb1 N4 74.65(11) . .
O2 Tb1 N6 75.67(10) . .
O1 Tb1 N6 70.76(10) . .
N3 Tb1 N6 75.23(10) . .
N1 Tb1 N6 136.60(12) . .
N4 Tb1 N6 119.86(11) . .
O2 Tb1 N9 143.59(9) . .
O1 Tb1 N9 85.12(10) . .
N3 Tb1 N9 74.60(10) . .
N1 Tb1 N9 71.38(11) . .
N4 Tb1 N9 143.25(10) . .
N6 Tb1 N9 78.38(11) . .
O2 Tb1 N7 81.57(10) . .
O1 Tb1 N7 142.35(9) . .
N3 Tb1 N7 74.00(10) . .
N1 Tb1 N7 74.79(12) . .
N4 Tb1 N7 76.07(10) . .
N6 Tb1 N7 145.61(10) . .
N9 Tb1 N7 107.50(11) . .
N3 C2 N2 175.6(4) 4_665 .
C3 N5 C4 121.9(3) . .
C3 N4 Tb1 148.7(3) . .
C1 N2 C2 118.7(3) . .
N6 C4 N5 173.0(4) 4_665 .
C1 N1 Tb1 177.8(3) . .
N1 C1 N2 174.6(4) . .
N4 C3 N5 174.6(4) . .
Tb1 O1 H1 120(3) . .
Tb1 O1 H2 129(3) . .
H1 O1 H2 106(3) . .
C4 N6 Tb1 159.8(3) 4_566 .
C5 N7 Tb1 154.0(3) . .
C2 N3 Tb1 156.2(3) 4_566 .
Tb1 O2 H3 121(3) . .
Tb1 O2 H4 128(3) . .
H3 O2 H4 107(3) . .
C6 N9 Tb1 160.5(3) . .
N9 C6 N8 173.4(4) . .
C5 N8 C6 120.7(3) 2_455 .
N7 C5 N8 174.0(4) . 2_445
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O2 2.371(2) .
Tb1 O1 2.381(3) .
Tb1 N3 2.439(3) .
Tb1 N1 2.444(3) .
Tb1 N4 2.457(3) .
Tb1 N6 2.469(3) .
Tb1 N9 2.469(3) .
Tb1 N7 2.481(3) .
C2 N3 1.145(4) 4_665
C2 N2 1.308(4) .
N5 C3 1.289(4) .
N5 C4 1.293(4) .
N4 C3 1.145(4) .
N2 C1 1.303(4) .
C4 N6 1.144(4) 4_665
N1 C1 1.139(4) .
O1 H1 0.860(18) .
O1 H2 0.867(18) .
N6 C4 1.144(4) 4_566
N7 C5 1.149(4) .
N3 C2 1.145(4) 4_566
O2 H3 0.862(18) .
O2 H4 0.847(18) .
N9 C6 1.137(4) .
C6 N8 1.310(5) .
N8 C5 1.300(4) 2_455
C5 N8 1.300(4) 2_445
