#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:34:46 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232734 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/80/4348083.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_4348083
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 Dy N2 O8'
_chemical_formula_weight         375.63
_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                   18.3308(5)
_cell_length_b                   6.5959(2)
_cell_length_c                   7.5993(2)
_cell_measurement_reflns_used    7370
_cell_measurement_temperature    290
_cell_measurement_theta_max      30.3490
_cell_measurement_theta_min      3.4620
_cell_volume                     918.82(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      290
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0280
_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            13571
_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    8.163
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.244
_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    2.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.548
_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   -0.027(12)
_refine_ls_extinction_coef       0.0038(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   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2097
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0171
_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)+(0.0168P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0386
_reflns_number_gt                2008
_reflns_number_total             2097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00952_si_002.cif
_cod_data_source_block           Dy-NH2NH3-290K
_cod_original_sg_symbol_H-M      'P ca2(1)'
_cod_database_code               4348083
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
Dy1 Dy 0.398004(7) 0.796040(19) 0.26609(4) 0.01283(6) Uani 1 1 d .
O1 O 0.42753(15) 0.5940(4) 0.5236(3) 0.0229(6) Uani 1 1 d .
O2 O 0.49474(15) 0.3950(5) 0.6928(3) 0.0249(6) Uani 1 1 d .
O3 O 0.32227(17) 0.8828(5) 0.4922(4) 0.0341(7) Uani 1 1 d .
O4 O 0.21966(18) 0.8055(4) 0.6275(5) 0.0362(8) Uani 1 1 d .
O5 O 0.34748(14) 0.4690(4) 0.2204(4) 0.0258(8) Uani 1 1 d .
O6 O 0.37523(18) 0.1437(4) 0.1933(4) 0.0285(7) Uani 1 1 d .
O7 O 0.49104(16) 0.9750(5) 0.4073(3) 0.0277(7) Uani 1 1 d .
O8 O 0.58531(17) 1.1774(4) 0.4583(4) 0.0226(6) Uani 1 1 d .
C1 C 0.4869(2) 0.5223(6) 0.5747(5) 0.0227(8) Uani 1 1 d .
H1 H 0.5289 0.5686 0.5191 0.027 Uiso 1 1 calc R
C2 C 0.2636(3) 0.9219(6) 0.5647(6) 0.0314(11) Uani 1 1 d .
H2 H 0.2516 1.0587 0.5720 0.038 Uiso 1 1 calc R
C3 C 0.3616(2) 0.2947(5) 0.2793(12) 0.0240(10) Uani 1 1 d .
H3 H 0.3617 0.2800 0.4011 0.029 Uiso 1 1 calc R
C4 C 0.5437(2) 1.0770(6) 0.3604(5) 0.0221(8) Uani 1 1 d .
H4 H 0.5537 1.0800 0.2405 0.027 Uiso 1 1 calc R
N1 N 0.32066(17) 0.5302(5) 0.7827(7) 0.0316(8) Uani 1 1 d D
H11 H 0.3292 0.6015 0.8800 0.047 Uiso 1 1 calc R
H12 H 0.2742 0.5452 0.7510 0.047 Uiso 1 1 calc R
H13 H 0.3495 0.5743 0.6966 0.047 Uiso 1 1 calc R
N2 N 0.3352(3) 0.3208(7) 0.8154(5) 0.0429(13) Uani 1 1 d D
H21 H 0.3769(19) 0.286(3) 0.764(7) 0.064 Uiso 1 1 d D
H22 H 0.339(3) 0.300(3) 0.9305(16) 0.064 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'
Dy Dy -0.1892 4.4098 '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 Dy1 O7 88.37(11) . .
O3 Dy1 O8 143.58(11) . 2_674
O7 Dy1 O8 108.82(10) . 2_674
O3 Dy1 O5 95.78(11) . .
O7 Dy1 O5 144.26(10) . .
O8 Dy1 O5 88.45(10) 2_674 .
O3 Dy1 O6 80.08(11) . 1_565
O7 Dy1 O6 75.50(11) . 1_565
O8 Dy1 O6 73.95(10) 2_674 1_565
O5 Dy1 O6 140.21(10) . 1_565
O3 Dy1 O2 143.57(10) . 2_664
O7 Dy1 O2 76.92(10) . 2_664
O8 Dy1 O2 72.75(10) 2_674 2_664
O5 Dy1 O2 78.96(9) . 2_664
O6 Dy1 O2 126.27(10) 1_565 2_664
O3 Dy1 O4 77.14(13) . 4_554
O7 Dy1 O4 147.62(10) . 4_554
O8 Dy1 O4 71.36(12) 2_674 4_554
O5 Dy1 O4 66.98(9) . 4_554
O6 Dy1 O4 73.58(10) 1_565 4_554
O2 Dy1 O4 130.35(11) 2_664 4_554
O3 Dy1 O1 70.52(10) . .
O7 Dy1 O1 75.18(10) . .
O8 Dy1 O1 143.95(10) 2_674 .
O5 Dy1 O1 72.91(9) . .
O6 Dy1 O1 138.60(10) 1_565 .
O2 Dy1 O1 73.53(9) 2_664 .
O4 Dy1 O1 124.61(10) 4_554 .
C1 O1 Dy1 130.7(3) . .
C1 O2 Dy1 128.3(3) . 2_665
C2 O3 Dy1 156.6(3) . .
C2 O4 Dy1 141.9(3) . 4
C3 O5 Dy1 134.2(3) . .
C3 O6 Dy1 134.0(4) . 1_545
C4 O7 Dy1 135.8(2) . .
C4 O8 Dy1 134.8(3) . 2_675
O2 C1 O1 125.7(4) . .
O2 C1 H1 117.2 . .
O1 C1 H1 117.2 . .
O4 C2 O3 128.5(4) . .
O4 C2 H2 115.7 . .
O3 C2 H2 115.7 . .
O6 C3 O5 126.7(8) . .
O6 C3 H3 116.6 . .
O5 C3 H3 116.6 . .
O7 C4 O8 126.5(4) . .
O7 C4 H4 116.8 . .
O8 C4 H4 116.8 . .
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 109.6(12) . .
N1 N2 H22 109.5(12) . .
H21 N2 H22 109.4(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O3 2.282(3) .
Dy1 O7 2.335(3) .
Dy1 O8 2.365(3) 2_674
Dy1 O5 2.373(3) .
Dy1 O6 2.395(3) 1_565
Dy1 O2 2.401(3) 2_664
Dy1 O4 2.401(3) 4_554
Dy1 O1 2.429(3) .
O1 C1 1.249(5) .
O2 C1 1.237(5) .
O2 Dy1 2.401(3) 2_665
O3 C2 1.235(5) .
O4 C2 1.211(5) .
O4 Dy1 2.401(3) 4
O5 C3 1.261(5) .
O6 C3 1.217(6) .
O6 Dy1 2.395(3) 1_545
O7 C4 1.230(5) .
O8 C4 1.254(5) .
O8 Dy1 2.365(3) 2_675
C1 H1 0.9300 .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 H4 0.9300 .
N1 N2 1.428(5) .
N1 H11 0.8900 .
N1 H12 0.8900 .
N1 H13 0.8900 .
N2 H21 0.889(10) .
N2 H22 0.887(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 0.93 2.56 3.094(5) 116.6 4_565
C4 H4 O7 0.93 2.69 3.519(5) 149.4 2_674
N1 H11 O4 0.89 2.48 3.273(6) 148.6 4
N1 H11 O8 0.89 2.22 2.911(5) 133.8 2_675
N1 H12 O4 0.89 2.20 2.849(5) 129.6 .
N1 H12 O5 0.89 2.30 3.144(4) 158.6 4
N1 H13 O1 0.89 1.95 2.809(5) 162.7 .
N1 H13 O3 0.89 2.61 3.207(6) 125.4 .
N2 H21 O2 0.889(10) 2.34(3) 3.108(5) 144(3) .
N2 H22 O5 0.887(10) 2.474(19) 3.237(5) 144.3(19) 1_556
N2 H22 O6 0.887(10) 2.346(14) 3.186(5) 158(3) 1_556
