#------------------------------------------------------------------------------
#$Date: 2019-11-28 18:37:24 +0100 (Thu 28 de Nov de 2019) $
#$Revision: 244418 $
#$URL: svn://www.crystallography.net/cod/cif/4/35/07/4350727.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_4350727
loop_
_publ_author_name
'Chen, Sa'
'Shang, Ran'
'Hu, Ke-Li'
'Wang, Zhe-Ming'
'Gao, Song'
_publ_section_title
;
 [NH2NH3][M(HCOO)3] (M = Mn2+, Zn2+, Co2+and Mg2+): structural phase
 transitions, prominent dielectric anomalies and negative thermal
 expansion, and magnetic ordering
;
_journal_issue                   1
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              83
_journal_paper_doi               10.1039/C3QI00034F
_journal_volume                  1
_journal_year                    2014
_chemical_formula_sum            'C3 H8 N2 O6 Zn'
_chemical_formula_weight         233.48
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n 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                   8.6806(3)
_cell_length_b                   7.7235(3)
_cell_length_c                   11.5056(3)
_cell_measurement_reflns_used    6249
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      28.700
_cell_measurement_theta_min      3.395
_cell_volume                     771.39(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_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, 1997)'
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14258
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         3.53
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.181
_exptl_absorpt_correction_T_max  0.471
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.322(12)
_refine_ls_extinction_coef       0.0461(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1965
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0227
_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)+(0.0181P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                1369
_reflns_number_total             1965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qi00034f.txt
_cod_data_source_block           2Zn-200K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P na2(1)'
_cod_database_code               4350727
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, 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
Zn1 Zn 0.52881(3) 0.49988(6) 0.11119(6) 0.01351(8) Uani 1 1 d .
O1 O 0.31458(19) 0.4204(2) 0.17709(17) 0.0197(4) Uani 1 1 d .
O2 O 0.12509(19) 0.2288(2) 0.17824(15) 0.0186(4) Uani 1 1 d .
O3 O 0.4308(2) 0.7257(2) 0.04127(15) 0.0202(4) Uani 1 1 d .
O4 O 0.23973(19) 0.9164(2) 0.04017(16) 0.0189(4) Uani 1 1 d .
O5 O 0.5554(2) 0.6421(3) 0.26656(14) 0.0186(5) Uani 1 1 d .
O6 O 0.5121(2) 0.6364(3) 0.45631(16) 0.0206(5) Uani 1 1 d .
C1 C 0.2591(3) 0.2770(4) 0.1518(2) 0.0207(7) Uani 1 1 d .
H1 H 0.3221 0.1985 0.1096 0.025 Uiso 1 1 calc R
C2 C 0.3112(3) 0.7897(4) 0.0824(2) 0.0203(7) Uani 1 1 d .
H2 H 0.2706 0.7387 0.1510 0.024 Uiso 1 1 calc R
C3 C 0.5306(3) 0.5628(3) 0.3618(3) 0.0203(8) Uani 1 1 d .
H3 H 0.5260 0.4400 0.3603 0.024 Uiso 1 1 calc R
N1 N 0.0636(4) 0.5065(3) 0.3433(3) 0.0203(8) Uani 1 1 d D
H11 H 0.0769 0.6137 0.3122 0.030 Uiso 1 1 calc R
H12 H 0.0754 0.4251 0.2868 0.030 Uiso 1 1 calc R
H13 H 0.1349 0.4888 0.4001 0.030 Uiso 1 1 calc R
N2 N -0.0883(5) 0.4935(3) 0.3920(3) 0.0316(9) Uani 1 1 d D
H21 H -0.112(2) 0.5916(17) 0.430(2) 0.047 Uiso 1 1 d D
H22 H -0.094(2) 0.401(2) 0.4398(19) 0.047 Uiso 1 1 d D
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.01475(12) 0.01247(12) 0.01331(11) 0.00011(11) 0.0008(2) 0.00007(15)
O1 0.0177(10) 0.0139(10) 0.0274(9) -0.0021(9) 0.0029(8) -0.0039(8)
O2 0.0184(11) 0.0172(10) 0.0202(8) -0.0025(8) 0.0041(8) -0.0039(8)
O3 0.0216(11) 0.0168(10) 0.0223(10) 0.0023(9) 0.0050(8) 0.0067(8)
O4 0.0204(10) 0.0162(10) 0.0201(9) 0.0016(9) 0.0031(8) 0.0037(8)
O5 0.0248(11) 0.0165(12) 0.0145(10) 0.0011(8) 0.0018(8) -0.0044(10)
O6 0.0331(12) 0.0158(12) 0.0129(10) -0.0007(9) 0.0035(8) -0.0019(10)
C1 0.0188(15) 0.0210(16) 0.0223(15) -0.0039(11) 0.0042(10) 0.0011(13)
C2 0.0215(15) 0.0198(16) 0.0195(16) 0.0007(11) 0.0011(10) 0.0032(13)
C3 0.022(3) 0.0187(11) 0.0202(12) -0.0014(15) -0.0040(14) -0.0020(12)
N1 0.0237(19) 0.0179(15) 0.0193(15) 0.0017(11) -0.0018(11) 0.0024(12)
N2 0.0236(19) 0.0316(19) 0.040(2) 0.0063(12) 0.0113(16) 0.0047(14)
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'
Zn Zn 0.2839 1.4301 '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
O6 Zn1 O1 90.56(7) 2_664 .
O6 Zn1 O2 87.56(8) 2_664 3
O1 Zn1 O2 88.50(7) . 3
O6 Zn1 O3 91.30(8) 2_664 .
O1 Zn1 O3 91.28(7) . .
O2 Zn1 O3 178.84(9) 3 .
O6 Zn1 O4 88.39(8) 2_664 3_565
O1 Zn1 O4 178.02(9) . 3_565
O2 Zn1 O4 93.14(7) 3 3_565
O3 Zn1 O4 87.06(7) . 3_565
O6 Zn1 O5 176.41(9) 2_664 .
O1 Zn1 O5 86.75(8) . .
O2 Zn1 O5 94.75(8) 3 .
O3 Zn1 O5 86.37(8) . .
O4 Zn1 O5 94.22(8) 3_565 .
C1 O1 Zn1 121.30(18) . .
C1 O2 Zn1 121.84(18) . 3_455
C2 O3 Zn1 121.50(16) . .
C2 O4 Zn1 121.21(17) . 3_465
C3 O5 Zn1 117.42(19) . .
C3 O6 Zn1 122.5(2) . 2_665
O1 C1 O2 124.4(3) . .
O1 C1 H1 117.8 . .
O2 C1 H1 117.8 . .
O3 C2 O4 125.1(2) . .
O3 C2 H2 117.5 . .
O4 C2 H2 117.5 . .
O6 C3 O5 123.9(2) . .
O6 C3 H3 118.1 . .
O5 C3 H3 118.1 . .
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 110.1(10) . .
N1 N2 H22 110.0(10) . .
H21 N2 H22 110.9(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O6 2.100(2) 2_664
Zn1 O1 2.1001(17) .
Zn1 O2 2.1009(19) 3
Zn1 O3 2.1010(19) .
Zn1 O4 2.1067(17) 3_565
Zn1 O5 2.111(2) .
O1 C1 1.242(3) .
O2 C1 1.259(3) .
O2 Zn1 2.1009(19) 3_455
O3 C2 1.243(3) .
O4 C2 1.256(3) .
O4 Zn1 2.1067(17) 3_465
O5 C3 1.274(4) .
O6 C3 1.237(4) .
O6 Zn1 2.100(2) 2_665
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 H3 0.9500 .
N1 N2 1.436(3) .
N1 H11 0.9100 .
N1 H12 0.9100 .
N1 H13 0.9100 .
N2 H21 0.901(9) .
N2 H22 0.905(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
N1 H11 O5 0.91 1.97 2.856(3) 165.1 3_465
N1 H11 O6 0.91 2.61 3.082(4) 113.3 3_465
N1 H12 O2 0.91 2.01 2.914(3) 171.3 .
N1 H12 O1 0.91 2.43 2.974(4) 118.5 .
N1 H13 O4 0.91 2.02 2.920(4) 168.2 4_545
N2 H21 O6 0.901(9) 2.381(15) 3.078(4) 134.3(12) 3_465
N2 H22 O3 0.905(9) 2.279(17) 3.016(3) 138.3(15) 4_545
