#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:34:46 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232734 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/80/4348080.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_4348080
loop_
_publ_author_name
'Zhao, Tian-Meng'
'Chen, Sa'
'Shang, Ran'
'Wang, Bing-Wu'
'Wang, Zhe-Ming'
'Gao, Song'
_publ_section_title
;
 Perovskite-Like Polar Lanthanide Formate Frameworks of
 [NH₂NH₃][Ln(HCOO)₄] (Ln = Tb-Lu and Y):
 Synthesis, Structures, Magnetism, and Anisotropic Thermal Expansion.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10075
_journal_page_last               10082
_journal_paper_doi               10.1021/acs.inorgchem.6b00952
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C4 H9 N2 O8 Tb'
_chemical_formula_weight         372.05
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_cell_setting           orthorhombic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2526(7)
_cell_length_b                   6.5815(2)
_cell_length_c                   7.6362(3)
_cell_measurement_reflns_used    5894
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      29.9360
_cell_measurement_theta_min      4.2110
_cell_volume                     917.33(6)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180.0
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13589
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.48
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.740
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2091
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0195
_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/[σ²(Fo²)+(0.0160P)²+1.1100P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0427
_reflns_number_gt                1965
_reflns_number_total             2091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00952_si_002.cif
_cod_data_source_block           Tb-NH2NH3-180K
_cod_original_sg_symbol_H-M      'P ca2(1)'
_cod_database_code               4348080
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, 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 0.398037(8) 0.80123(2) 0.26678(5) 0.00945(6) Uani 1 1 d .
O1 O 0.42838(19) 0.5927(5) 0.5174(4) 0.0167(7) Uani 1 1 d .
O2 O 0.49436(18) 0.3899(5) 0.6903(4) 0.0176(7) Uani 1 1 d .
O3 O 0.3241(2) 0.8869(6) 0.4993(5) 0.0242(8) Uani 1 1 d .
O4 O 0.2219(2) 0.8196(6) 0.6412(6) 0.0313(10) Uani 1 1 d .
O5 O 0.34511(17) 0.4747(5) 0.2210(4) 0.0198(9) Uani 1 1 d .
O6 O 0.3774(2) 0.1502(5) 0.1945(5) 0.0220(8) Uani 1 1 d .
O7 O 0.4929(2) 0.9762(5) 0.4103(4) 0.0201(8) Uani 1 1 d .
O8 O 0.5888(2) 1.1785(5) 0.4579(5) 0.0171(7) Uani 1 1 d .
C1 C 0.4880(3) 0.5182(7) 0.5702(6) 0.0152(10) Uani 1 1 d .
H1 H 0.5316 0.5631 0.5145 0.018 Uiso 1 1 calc R
C2 C 0.2633(3) 0.9293(8) 0.5613(6) 0.0223(13) Uani 1 1 d .
H2 H 0.2471 1.0650 0.5440 0.027 Uiso 1 1 calc R
C3 C 0.3599(2) 0.2995(6) 0.2807(15) 0.0185(12) Uani 1 1 d .
H3 H 0.3571 0.2825 0.4041 0.022 Uiso 1 1 calc R
C4 C 0.5459(3) 1.0787(7) 0.3602(6) 0.0153(10) Uani 1 1 d .
H4 H 0.5551 1.0828 0.2378 0.018 Uiso 1 1 calc R
N1 N 0.32144(19) 0.5350(5) 0.7749(9) 0.0200(8) Uani 1 1 d D
H11 H 0.3348 0.6153 0.8665 0.030 Uiso 1 1 calc R
H12 H 0.2728 0.5513 0.7532 0.030 Uiso 1 1 calc R
H13 H 0.3476 0.5706 0.6782 0.030 Uiso 1 1 calc R
N2 N 0.3360(3) 0.3254(7) 0.8175(6) 0.0275(12) Uani 1 1 d D
H21 H 0.3816(16) 0.291(4) 0.778(7) 0.041 Uiso 1 1 d D
H22 H 0.335(3) 0.309(3) 0.9362(17) 0.041 Uiso 1 1 d 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
O3 Tb1 O7 87.26(13) . .
O3 Tb1 O8 144.31(13) . 2_674
O7 Tb1 O8 111.15(12) . 2_674
O3 Tb1 O5 95.55(13) . .
O7 Tb1 O5 144.03(11) . .
O8 Tb1 O5 86.90(11) 2_674 .
O3 Tb1 O6 81.38(13) . 1_565
O7 Tb1 O6 75.72(13) . 1_565
O8 Tb1 O6 74.49(12) 2_674 1_565
O5 Tb1 O6 140.21(12) . 1_565
O3 Tb1 O4 76.13(15) . 4_554
O7 Tb1 O4 146.72(13) . 4_554
O8 Tb1 O4 72.04(14) 2_674 4_554
O5 Tb1 O4 67.39(11) . 4_554
O6 Tb1 O4 73.43(13) 1_565 4_554
O3 Tb1 O2 142.66(12) . 2_664
O7 Tb1 O2 76.58(12) . 2_664
O8 Tb1 O2 72.87(12) 2_674 2_664
O5 Tb1 O2 79.84(11) . 2_664
O6 Tb1 O2 125.11(12) 1_565 2_664
O4 Tb1 O2 132.55(13) 4_554 2_664
O3 Tb1 O1 70.30(12) . .
O7 Tb1 O1 74.97(11) . .
O8 Tb1 O1 142.60(12) 2_674 .
O5 Tb1 O1 72.37(11) . .
O6 Tb1 O1 139.77(12) 1_565 .
O4 Tb1 O1 123.71(12) 4_554 .
O2 Tb1 O1 73.04(11) 2_664 .
C1 O1 Tb1 132.2(3) . .
C1 O2 Tb1 127.3(3) . 2_665
C2 O3 Tb1 151.2(3) . .
C2 O4 Tb1 143.4(4) . 4
C3 O5 Tb1 132.9(4) . .
C3 O6 Tb1 133.4(5) . 1_545
C4 O7 Tb1 134.2(3) . .
C4 O8 Tb1 132.7(3) . 2_675
O2 C1 O1 125.2(4) . .
O2 C1 H1 117.4 . .
O1 C1 H1 117.4 . .
O4 C2 O3 128.1(5) . .
O4 C2 H2 115.9 . .
O3 C2 H2 115.9 . .
O6 C3 O5 126.2(10) . .
O6 C3 H3 116.9 . .
O5 C3 H3 116.9 . .
O7 C4 O8 125.7(4) . .
O7 C4 H4 117.2 . .
O8 C4 H4 117.2 . .
N2 N1 H11 109.5 . .
N2 N1 H12 109.5 . .
H11 N1 H12 109.5 . .
N2 N1 H13 109.5 . .
H11 N1 H13 109.5 . .
H12 N1 H13 109.5 . .
N1 N2 H21 109.2(12) . .
N1 N2 H22 109.4(12) . .
H21 N2 H22 108.9(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O3 2.300(3) .
Tb1 O7 2.351(3) .
Tb1 O8 2.374(3) 2_674
Tb1 O5 2.382(3) .
Tb1 O6 2.392(3) 1_565
Tb1 O4 2.394(4) 4_554
Tb1 O2 2.405(3) 2_664
Tb1 O1 2.419(3) .
O1 C1 1.260(6) .
O2 C1 1.252(6) .
O2 Tb1 2.405(3) 2_665
O3 C2 1.239(6) .
O4 C2 1.210(6) .
O4 Tb1 2.394(4) 4
O5 C3 1.269(6) .
O6 C3 1.225(8) .
O6 Tb1 2.392(3) 1_545
O7 C4 1.240(6) .
O8 C4 1.265(6) .
O8 Tb1 2.374(3) 2_675
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 H4 0.9500 .
N1 N2 1.442(6) .
N1 H11 0.9100 .
N1 H12 0.9100 .
N1 H13 0.9100 .
N2 H21 0.915(10) .
N2 H22 0.913(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2 O6 0.95 2.61 3.121(6) 114.3 4_565
C4 H4 O7 0.95 2.68 3.526(6) 149.0 2_674
N1 H11 O4 0.91 2.70 3.458(8) 141.6 4
N1 H11 O8 0.91 2.07 2.863(6) 145.3 2_675
N1 H12 O4 0.91 2.17 2.802(5) 125.8 .
N1 H12 O5 0.91 2.22 3.093(5) 159.7 4
N1 H13 O1 0.91 1.92 2.797(7) 159.9 .
N1 H13 O3 0.91 2.53 3.130(7) 124.2 .
N2 H21 O2 0.915(10) 2.26(2) 3.079(6) 149(2) .
N2 H22 O5 0.913(10) 2.44(2) 3.238(5) 146(3) 1_556
N2 H22 O6 0.913(10) 2.36(2) 3.192(5) 151(3) 1_556
