#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:34:46 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232734 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/80/4348084.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_4348084
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 Ho N2 O8'
_chemical_formula_weight         378.06
_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                   18.2209(5)
_cell_length_b                   6.5751(2)
_cell_length_c                   7.5850(2)
_cell_measurement_reflns_used    9091
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      30.0530
_cell_measurement_theta_min      4.2310
_cell_volume                     908.72(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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0284
_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            13200
_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    8.738
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.177
_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            'pale pink'
_exptl_crystal_density_diffrn    2.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(12)
_refine_ls_extinction_coef       0.0026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2070
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0185
_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)+(0.0184P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0417
_reflns_number_gt                1999
_reflns_number_total             2070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00952_si_002.cif
_cod_data_source_block           Ho-NH2NH3-180K
_cod_original_sg_symbol_H-M      'P ca2(1)'
_cod_database_code               4348084
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
Ho1 Ho 0.397953(7) 0.79568(2) 0.26603(4) 0.00899(7) Uani 1 1 d .
O1 O 0.42679(17) 0.5940(4) 0.5232(4) 0.0156(6) Uani 1 1 d .
O2 O 0.49413(16) 0.3941(5) 0.6947(4) 0.0169(6) Uani 1 1 d .
O3 O 0.32209(18) 0.8852(5) 0.4906(4) 0.0230(7) Uani 1 1 d .
O4 O 0.21905(18) 0.8057(5) 0.6262(5) 0.0271(8) Uani 1 1 d .
O5 O 0.34694(15) 0.4690(4) 0.2218(4) 0.0190(8) Uani 1 1 d .
O6 O 0.37634(18) 0.1427(5) 0.1913(4) 0.0183(7) Uani 1 1 d .
O7 O 0.49067(17) 0.9728(5) 0.4086(4) 0.0196(7) Uani 1 1 d .
O8 O 0.58496(19) 1.1797(4) 0.4600(4) 0.0164(7) Uani 1 1 d .
C1 C 0.4869(2) 0.5228(7) 0.5757(5) 0.0153(8) Uani 1 1 d .
H1 H 0.5303 0.5711 0.5202 0.018 Uiso 1 1 calc R
C2 C 0.2640(2) 0.9244(7) 0.5671(6) 0.0208(10) Uani 1 1 d .
H2 H 0.2529 1.0646 0.5815 0.025 Uiso 1 1 calc R
C3 C 0.3621(2) 0.2922(5) 0.2801(12) 0.0184(10) Uani 1 1 d .
H3 H 0.3622 0.2751 0.4044 0.022 Uiso 1 1 calc R
C4 C 0.5439(2) 1.0783(6) 0.3598(5) 0.0153(9) Uani 1 1 d .
H4 H 0.5542 1.0823 0.2371 0.018 Uiso 1 1 calc R
N1 N 0.31969(18) 0.5305(5) 0.7805(7) 0.0215(8) Uani 1 1 d D
H11 H 0.3339 0.6091 0.8732 0.032 Uiso 1 1 calc R
H12 H 0.2706 0.5453 0.7629 0.032 Uiso 1 1 calc R
H13 H 0.3443 0.5698 0.6818 0.032 Uiso 1 1 calc R
N2 N 0.3359(3) 0.3207(6) 0.8180(5) 0.0273(10) Uani 1 1 d D
H21 H 0.3832(13) 0.293(3) 0.784(7) 0.041 Uiso 1 1 d D
H22 H 0.332(3) 0.297(3) 0.936(2) 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'
Ho Ho -0.2175 4.6783 '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 Ho1 O7 87.90(11) . .
O3 Ho1 O8 143.56(12) . 2_674
O7 Ho1 O8 109.26(11) . 2_674
O3 Ho1 O5 95.89(11) . .
O7 Ho1 O5 143.96(10) . .
O8 Ho1 O5 88.54(10) 2_674 .
O3 Ho1 O4 77.41(13) . 4_554
O7 Ho1 O4 147.73(11) . 4_554
O8 Ho1 O4 71.13(12) 2_674 4_554
O5 Ho1 O4 67.05(10) . 4_554
O3 Ho1 O6 80.20(11) . 1_565
O7 Ho1 O6 75.56(11) . 1_565
O8 Ho1 O6 73.78(10) 2_674 1_565
O5 Ho1 O6 140.43(11) . 1_565
O4 Ho1 O6 73.72(11) 4_554 1_565
O3 Ho1 O2 143.66(11) . 2_664
O7 Ho1 O2 76.62(10) . 2_664
O8 Ho1 O2 72.72(11) 2_674 2_664
O5 Ho1 O2 79.46(10) . 2_664
O4 Ho1 O2 130.52(11) 4_554 2_664
O6 Ho1 O2 125.56(11) 1_565 2_664
O3 Ho1 O1 70.67(11) . .
O7 Ho1 O1 74.97(10) . .
O8 Ho1 O1 143.82(10) 2_674 .
O5 Ho1 O1 72.64(10) . .
O4 Ho1 O1 124.69(11) 4_554 .
O6 Ho1 O1 138.86(10) 1_565 .
O2 Ho1 O1 73.60(10) 2_664 .
C1 O1 Ho1 130.5(3) . .
C1 O2 Ho1 127.3(3) . 2_665
C2 O3 Ho1 158.2(3) . .
C2 O4 Ho1 141.6(3) . 4
C3 O5 Ho1 134.0(3) . .
C3 O6 Ho1 132.5(4) . 1_545
C4 O7 Ho1 135.0(3) . .
C4 O8 Ho1 135.5(3) . 2_675
O2 C1 O1 125.2(4) . .
O2 C1 H1 117.4 . .
O1 C1 H1 117.4 . .
O4 C2 O3 128.1(4) . .
O4 C2 H2 116.0 . .
O3 C2 H2 116.0 . .
O6 C3 O5 126.2(8) . .
O6 C3 H3 116.9 . .
O5 C3 H3 116.9 . .
O7 C4 O8 125.3(4) . .
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 109.1(11) . .
N1 N2 H22 109.8(12) . .
H21 N2 H22 108.8(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O3 2.271(3) .
Ho1 O7 2.319(3) .
Ho1 O8 2.348(3) 2_674
Ho1 O5 2.364(3) .
Ho1 O4 2.382(3) 4_554
Ho1 O6 2.384(3) 1_565
Ho1 O2 2.391(3) 2_664
Ho1 O1 2.417(3) .
O1 C1 1.256(5) .
O2 C1 1.244(5) .
O2 Ho1 2.391(3) 2_665
O3 C2 1.234(5) .
O4 C2 1.216(5) .
O4 Ho1 2.382(3) 4
O5 C3 1.274(5) .
O6 C3 1.220(6) .
O6 Ho1 2.384(3) 1_545
O7 C4 1.249(5) .
O8 C4 1.257(5) .
O8 Ho1 2.348(3) 2_675
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 H4 0.9500 .
N1 N2 1.439(5) .
N1 H11 0.9100 .
N1 H12 0.9100 .
N1 H13 0.9100 .
N2 H21 0.918(10) .
N2 H22 0.911(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 3.080(6) 115.3 4_565
C4 H4 O7 0.95 2.65 3.496(5) 149.0 2_674
N1 H11 O4 0.91 2.51 3.263(7) 140.7 4
N1 H11 O8 0.91 2.13 2.916(5) 143.7 2_675
N1 H12 O4 0.91 2.21 2.830(5) 124.7 .
N1 H12 O5 0.91 2.22 3.095(4) 160.8 4
N1 H13 O1 0.91 1.93 2.791(5) 156.8 .
N1 H13 O3 0.91 2.56 3.206(6) 128.1 .
N2 H21 O2 0.918(10) 2.234(18) 3.070(6) 151.1(18) .
N2 H22 O5 0.911(10) 2.46(3) 3.221(5) 141(3) 1_556
N2 H22 O6 0.911(10) 2.33(2) 3.151(5) 149(3) 1_556
