#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:34:46 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232734 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/80/4348089.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_4348089
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 Tm'
_chemical_formula_weight         382.06
_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                   18.1409(5)
_cell_length_b                   6.5415(2)
_cell_length_c                   7.5452(2)
_cell_measurement_reflns_used    8794
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      30.2110
_cell_measurement_theta_min      4.2470
_cell_volume                     895.38(4)
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13686
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.51
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.940
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_correction_T_min  0.115
_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    2.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(11)
_refine_ls_extinction_coef       0.0123(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2209
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0171P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0421
_reflns_number_gt                2126
_reflns_number_total             2209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00952_si_002.cif
_cod_data_source_block           Tm-NH2NH3-180K
_cod_original_sg_symbol_H-M      'P ca2(1)'
_cod_database_code               4348089
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
Tm1 Tm 0.397934(7) 0.794405(18) 0.26604(4) 0.00840(6) Uani 1 1 d .
O1 O 0.42678(17) 0.5935(4) 0.5221(4) 0.0150(6) Uani 1 1 d .
O2 O 0.49489(16) 0.3938(4) 0.6941(3) 0.0163(6) Uani 1 1 d .
O3 O 0.32213(18) 0.8832(5) 0.4893(4) 0.0226(7) Uani 1 1 d .
O4 O 0.2183(2) 0.8039(4) 0.6248(5) 0.0264(8) Uani 1 1 d .
O5 O 0.34776(15) 0.4677(4) 0.2210(4) 0.0173(8) Uani 1 1 d .
O6 O 0.37609(19) 0.1391(5) 0.1930(4) 0.0184(6) Uani 1 1 d .
O7 O 0.48964(17) 0.9725(4) 0.4096(3) 0.0174(6) Uani 1 1 d .
O8 O 0.5844(2) 1.1793(4) 0.4612(4) 0.0156(7) Uani 1 1 d .
C1 C 0.4875(3) 0.5243(6) 0.5750(5) 0.0158(8) Uani 1 1 d .
H1 H 0.5309 0.5751 0.5203 0.019 Uiso 1 1 calc R
C2 C 0.2641(3) 0.9225(6) 0.5660(6) 0.0211(10) Uani 1 1 d .
H2 H 0.2535 1.0636 0.5816 0.025 Uiso 1 1 calc R
C3 C 0.3623(2) 0.2935(5) 0.2829(11) 0.0159(10) Uani 1 1 d .
H3 H 0.3628 0.2790 0.4081 0.019 Uiso 1 1 calc R
C4 C 0.5431(2) 1.0773(5) 0.3610(5) 0.0140(8) Uani 1 1 d .
H4 H 0.5536 1.0806 0.2377 0.017 Uiso 1 1 calc R
N1 N 0.31971(18) 0.5290(5) 0.7819(7) 0.0194(7) Uani 1 1 d D
H11 H 0.3295 0.6049 0.8801 0.029 Uiso 1 1 calc R
H12 H 0.2713 0.5424 0.7527 0.029 Uiso 1 1 calc R
H13 H 0.3482 0.5734 0.6903 0.029 Uiso 1 1 calc R
N2 N 0.3357(3) 0.3177(6) 0.8173(5) 0.0244(10) Uani 1 1 d D
H21 H 0.3833(12) 0.290(3) 0.790(7) 0.037 Uiso 1 1 d D
H22 H 0.327(3) 0.289(3) 0.933(3) 0.037 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'
Tm Tm -0.3139 5.2483 '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 Tm1 O7 87.64(11) . .
O3 Tm1 O8 143.52(12) . 2_674
O7 Tm1 O8 109.15(11) . 2_674
O3 Tm1 O5 96.11(11) . .
O7 Tm1 O5 144.02(10) . .
O8 Tm1 O5 88.71(10) 2_674 .
O3 Tm1 O6 79.94(11) . 1_565
O7 Tm1 O6 75.35(11) . 1_565
O8 Tm1 O6 73.80(10) 2_674 1_565
O5 Tm1 O6 140.58(11) . 1_565
O3 Tm1 O4 77.63(14) . 4_554
O7 Tm1 O4 147.53(10) . 4_554
O8 Tm1 O4 71.03(13) 2_674 4_554
O5 Tm1 O4 67.22(9) . 4_554
O6 Tm1 O4 73.68(10) 1_565 4_554
O3 Tm1 O2 143.96(10) . 2_664
O7 Tm1 O2 77.13(10) . 2_664
O8 Tm1 O2 72.47(11) 2_674 2_664
O5 Tm1 O2 79.14(10) . 2_664
O6 Tm1 O2 125.67(10) 1_565 2_664
O4 Tm1 O2 130.07(11) 4_554 2_664
O3 Tm1 O1 70.82(11) . .
O7 Tm1 O1 74.95(10) . .
O8 Tm1 O1 143.85(10) 2_674 .
O5 Tm1 O1 72.66(9) . .
O6 Tm1 O1 138.70(10) 1_565 .
O4 Tm1 O1 124.99(11) 4_554 .
O2 Tm1 O1 73.72(9) 2_664 .
C1 O1 Tm1 130.3(3) . .
C1 O2 Tm1 127.7(3) . 2_665
C2 O3 Tm1 158.4(3) . .
C2 O4 Tm1 142.0(3) . 4
C3 O5 Tm1 133.5(3) . .
C3 O6 Tm1 133.2(4) . 1_545
C4 O7 Tm1 134.8(3) . .
C4 O8 Tm1 135.7(3) . 2_675
O2 C1 O1 124.8(4) . .
O2 C1 H1 117.6 . .
O1 C1 H1 117.6 . .
O4 C2 O3 128.5(4) . .
O4 C2 H2 115.8 . .
O3 C2 H2 115.8 . .
O6 C3 O5 125.1(7) . .
O6 C3 H3 117.4 . .
O5 C3 H3 117.4 . .
O7 C4 O8 125.5(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 110.2(12) . .
N1 N2 H22 109.9(12) . .
H21 N2 H22 110.6(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tm1 O3 2.251(3) .
Tm1 O7 2.302(3) .
Tm1 O8 2.329(3) 2_674
Tm1 O5 2.348(3) .
Tm1 O6 2.355(3) 1_565
Tm1 O4 2.363(3) 4_554
Tm1 O2 2.364(3) 2_664
Tm1 O1 2.394(3) .
O1 C1 1.255(5) .
O2 C1 1.247(5) .
O2 Tm1 2.364(3) 2_665
O3 C2 1.229(5) .
O4 C2 1.220(5) .
O4 Tm1 2.363(3) 4
O5 C3 1.259(5) .
O6 C3 1.242(6) .
O6 Tm1 2.355(3) 1_545
O7 C4 1.243(5) .
O8 C4 1.256(5) .
O8 Tm1 2.329(3) 2_675
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 H4 0.9500 .
N1 N2 1.437(5) .
N1 H11 0.9100 .
N1 H12 0.9100 .
N1 H13 0.9100 .
N2 H21 0.907(10) .
N2 H22 0.907(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 2.55 3.065(6) 114.6 4_565
C4 H4 O7 0.95 2.62 3.473(5) 149.6 2_674
N1 H11 O4 0.91 2.42 3.225(6) 147.7 4
N1 H11 O8 0.91 2.19 2.915(5) 135.9 2_675
N1 H12 O4 0.91 2.19 2.833(5) 127.4 .
N1 H12 O5 0.91 2.23 3.099(4) 160.2 4
N1 H13 O1 0.91 1.91 2.792(5) 161.5 .
N1 H13 O3 0.91 2.58 3.201(5) 126.5 .
N2 H21 O2 0.907(10) 2.255(16) 3.074(6) 150.1(15) .
N2 H22 O5 0.907(10) 2.50(3) 3.207(5) 135(3) 1_556
N2 H22 O6 0.907(10) 2.37(3) 3.152(5) 144(4) 1_556
