#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:34:46 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232734 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/80/4348096.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_4348096
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 Y'
_chemical_formula_weight         302.04
_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                   18.2232(5)
_cell_length_b                   6.5790(2)
_cell_length_c                   7.5847(2)
_cell_measurement_reflns_used    7704
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      30.1250
_cell_measurement_theta_min      4.2230
_cell_volume                     909.33(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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0254
_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            13989
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.445
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.346
_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    2.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.034(5)
_refine_ls_extinction_coef       0.0024(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2072
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0189
_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)+(0.0179P)²+0.3040P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0419
_reflns_number_gt                1971
_reflns_number_total             2072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00952_si_002.cif
_cod_data_source_block           Y-NH2NH3-180K
_cod_original_sg_symbol_H-M      'P ca2(1)'
_cod_database_code               4348096
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
Y1 Y 0.397849(9) 0.79443(3) 0.26586(3) 0.00857(7) Uani 1 1 d .
O1 O 0.42647(9) 0.5950(2) 0.5237(2) 0.0147(4) Uani 1 1 d .
O2 O 0.49448(9) 0.3957(3) 0.6951(2) 0.0167(4) Uani 1 1 d .
O3 O 0.32158(10) 0.8856(3) 0.4892(2) 0.0231(4) Uani 1 1 d .
O4 O 0.21844(10) 0.8032(3) 0.6230(3) 0.0245(4) Uani 1 1 d .
O5 O 0.34751(8) 0.4679(2) 0.2223(2) 0.0163(4) Uani 1 1 d .
O6 O 0.37566(10) 0.1414(3) 0.1919(2) 0.0181(4) Uani 1 1 d .
O7 O 0.49037(9) 0.9730(3) 0.4076(2) 0.0169(4) Uani 1 1 d .
O8 O 0.58415(10) 1.1807(2) 0.4600(2) 0.0154(4) Uani 1 1 d .
C1 C 0.48706(14) 0.5248(4) 0.5754(3) 0.0149(5) Uani 1 1 d .
H1 H 0.5303 0.5735 0.5195 0.018 Uiso 1 1 calc R
C2 C 0.26405(14) 0.9234(4) 0.5693(3) 0.0199(6) Uani 1 1 d .
H2 H 0.2543 1.0629 0.5916 0.024 Uiso 1 1 calc R
C3 C 0.36244(12) 0.2932(3) 0.2825(5) 0.0162(5) Uani 1 1 d .
H3 H 0.3636 0.2776 0.4070 0.019 Uiso 1 1 calc R
C4 C 0.54356(13) 1.0779(3) 0.3595(3) 0.0137(5) Uani 1 1 d .
H4 H 0.5544 1.0806 0.2370 0.016 Uiso 1 1 calc R
N1 N 0.31963(11) 0.5299(3) 0.7812(4) 0.0200(4) Uani 1 1 d D
H11 H 0.3284 0.6062 0.8791 0.030 Uiso 1 1 calc R
H12 H 0.2716 0.5418 0.7500 0.030 Uiso 1 1 calc R
H13 H 0.3485 0.5744 0.6913 0.030 Uiso 1 1 calc R
N2 N 0.33609(13) 0.3200(3) 0.8182(3) 0.0261(6) Uani 1 1 d D
H21 H 0.3821(9) 0.292(2) 0.777(4) 0.039 Uiso 1 1 d D
H22 H 0.3354(17) 0.301(3) 0.9377(14) 0.039 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'
Y Y -2.7962 3.5667 '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 Y1 O7 88.01(7) . .
O3 Y1 O8 143.48(6) . 2_674
O7 Y1 O8 108.73(6) . 2_674
O3 Y1 O5 96.13(6) . .
O7 Y1 O5 143.99(6) . .
O8 Y1 O5 88.82(6) 2_674 .
O3 Y1 O4 77.77(7) . 4_554
O7 Y1 O4 147.75(6) . 4_554
O8 Y1 O4 70.93(7) 2_674 4_554
O5 Y1 O4 67.18(6) . 4_554
O3 Y1 O6 79.58(6) . 1_565
O7 Y1 O6 75.37(6) . 1_565
O8 Y1 O6 74.02(6) 2_674 1_565
O5 Y1 O6 140.59(6) . 1_565
O4 Y1 O6 73.67(6) 4_554 1_565
O3 Y1 O2 143.96(6) . 2_664
O7 Y1 O2 76.84(6) . 2_664
O8 Y1 O2 72.52(6) 2_674 2_664
O5 Y1 O2 79.11(6) . 2_664
O4 Y1 O2 129.92(7) 4_554 2_664
O6 Y1 O2 125.99(6) 1_565 2_664
O3 Y1 O1 70.81(6) . .
O7 Y1 O1 75.08(6) . .
O8 Y1 O1 143.95(6) 2_674 .
O5 Y1 O1 72.68(5) . .
O4 Y1 O1 125.07(6) 4_554 .
O6 Y1 O1 138.41(6) 1_565 .
O2 Y1 O1 73.72(6) 2_664 .
C1 O1 Y1 129.92(16) . .
C1 O2 Y1 127.44(16) . 2_665
C2 O3 Y1 159.71(18) . .
C2 O4 Y1 140.88(17) . 4
C3 O5 Y1 133.84(15) . .
C3 O6 Y1 132.50(19) . 1_545
C4 O7 Y1 135.31(15) . .
C4 O8 Y1 135.85(16) . 2_675
O2 C1 O1 124.8(2) . .
O2 C1 H1 117.6 . .
O1 C1 H1 117.6 . .
O4 C2 O3 127.8(2) . .
O4 C2 H2 116.1 . .
O3 C2 H2 116.1 . .
O6 C3 O5 125.1(3) . .
O6 C3 H3 117.5 . .
O5 C3 H3 117.5 . .
O7 C4 O8 125.3(2) . .
O7 C4 H4 117.4 . .
O8 C4 H4 117.4 . .
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 108.6(10) . .
N1 N2 H22 108.8(10) . .
H21 N2 H22 108.7(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Y1 O3 2.2716(17) .
Y1 O7 2.3195(17) .
Y1 O8 2.3482(18) 2_674
Y1 O5 2.3592(15) .
Y1 O4 2.3806(18) 4_554
Y1 O6 2.3851(17) 1_565
Y1 O2 2.3880(16) 2_664
Y1 O1 2.4119(16) .
O1 C1 1.259(3) .
O2 C1 1.250(3) .
O2 Y1 2.3880(16) 2_665
O3 C2 1.237(3) .
O4 C2 1.218(3) .
O4 Y1 2.3806(18) 4
O5 C3 1.266(3) .
O6 C3 1.236(3) .
O6 Y1 2.3851(17) 1_545
O7 C4 1.245(3) .
O8 C4 1.259(3) .
O8 Y1 2.3482(18) 2_675
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 H4 0.9500 .
N1 N2 1.441(3) .
N1 H11 0.9100 .
N1 H12 0.9100 .
N1 H13 0.9100 .
N2 H21 0.913(9) .
N2 H22 0.915(9) .
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 2.54 3.067(3) 115.1 4_565
C4 H4 O7 0.95 2.65 3.499(3) 148.7 2_674
N1 H11 O4 0.91 2.41 3.230(3) 149.2 4
N1 H11 O8 0.91 2.21 2.922(3) 134.6 2_675
N1 H12 O4 0.91 2.20 2.841(3) 127.3 .
N1 H12 O5 0.91 2.23 3.105(3) 160.0 4
N1 H13 O1 0.91 1.91 2.791(3) 162.1 .
N1 H13 O3 0.91 2.60 3.222(3) 125.8 .
N2 H22 O5 0.915(9) 2.433(17) 3.223(3) 144.6(16) 1_556
N2 H22 O6 0.915(9) 2.314(11) 3.152(3) 152.1(17) 1_556
N2 H21 O2 0.913(9) 2.247(15) 3.074(3) 150.4(16) .
