#------------------------------------------------------------------------------
#$Date: 2019-11-17 15:32:33 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230902 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/14/7231415.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_7231415
loop_
_publ_author_name
'Collings, Ines E.'
'Manna, Rudra Sekhar'
'Tsirlin, Alexander A.'
'Bykov, Maxim'
'Bykova, Elena'
'Hanfland, Michael'
'Gegenwart, Philipp'
'van Smaalen, Sander'
'Dubrovinsky, Leonid'
'Dubrovinskaia, Natalia'
_publ_section_title
;
 Pressure dependence of spin canting in ammonium metal formate
 antiferromagnets.
;
_journal_issue                   37
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              24465
_journal_page_last               24476
_journal_paper_doi               10.1039/c8cp03761b
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C3 H3 Ni O6, N H4'
_chemical_formula_sum            'C3 H7 N Ni O6'
_chemical_formula_weight         211.81
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_Hall           'P 6c 2c'
_space_group_name_H-M_alt        'P 63 2 2'
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-08-09 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   7.1831(2)
_cell_length_b                   7.1831(2)
_cell_length_c                   8.0511(2)
_cell_measurement_reflns_used    412
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.0000
_cell_measurement_theta_min      1.8950
_cell_volume                     359.757(17)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_pressure         '0.82 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.767
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41128
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.767
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1045
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.709
_diffrn_reflns_theta_full        14.286
_diffrn_reflns_theta_max         19.558
_diffrn_reflns_theta_min         1.894
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 90 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         395
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0147P)²+0.2027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.381
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.592
_reflns_number_gt                351
_reflns_number_total             395
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cp03761b2.cif
_cod_data_source_block           ANiF_c2_p04
_cod_depositor_comments
'Adding full bibliography for 7231402--7231432.cif.'
_cod_original_cell_volume        359.76(2)
_cod_database_code               7231415
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_res_file
;
TITL ANiF_c2_p04_s in P6(3)22
    ANiF_c2_p04_s.res
    created by SHELXL-2016/6 at 14:14:32 on 14-May-2017
REM P6(3)22 (#182 in standard setting)
CELL 0.41128   7.183116   7.183116   8.051121  90.0000  90.0000 120.0000
ZERR    2.00   0.000197   0.000197   0.000231   0.0000   0.0000   0.0000
LATT -1
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM -x,-y, z+1/2
SYMM  y,-x+y, z+1/2
SYMM  x-y, x, z+1/2
SYMM  y, x,-z
SYMM  x-y,-y,-z
SYMM -x,-x+y,-z
SYMM -y,-x,-z+1/2
SYMM -x+y, y,-z+1/2
SYMM  x, x-y,-z+1/2
SFAC C H N O Ni
DISP $C -0.00005  0.00048  5.14312!source kissel
DISP $H -0.00003  0.00000  0.64132!source kissel
DISP $N  0.00062  0.00099  7.19459!source kissel
DISP $O  0.00180  0.00183 10.16238!source kissel
DISP $Ni  0.23093  0.40937 987.78852!source kissel
UNIT 6.00 14.00 2.00 12.00 2.00
OMIT -1 2 2
OMIT 0 1 1
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
ACTA
BOND
FMAP 2
PLAN 20
WGHT    0.014700    0.202700
FVAR       9.03398
MOLE   1
NI1   5    0.333333    0.666667    0.250000    10.16667    0.02827    0.02827 =
         0.01549    0.00000    0.00000    0.01413
O1    4    0.309138    0.890760    0.106931    11.00000    0.04169    0.03833 =
         0.02953    0.01202    0.01014    0.02188
C1    1    0.441379    1.000000    0.000000    10.50000    0.03335    0.04984 =
         0.04134    0.02238    0.01119    0.02492
AFIX  43
H1    2    0.570850    1.000001    0.000003    10.50000   -1.20000
MOLE   2
REM #####
AFIX   0
N1    3    0.000000    1.000000    0.250000    10.16667    0.03821    0.03821 =
         0.09277    0.00000    0.00000    0.01910
DFIX 0.9 0.1 N1 H2
H2    2    0.085396    1.118430    0.310110    10.66667   -1.20000
HKLF 4




REM  ANiF_c2_p04_s in P6(3)22
REM R1 =  0.0315 for     351 Fo > 4sig(Fo)  and  0.0379 for all     395 data
REM     22 parameters refined using      0 restraints

END

WGHT      0.0147      0.2027

REM Highest difference peak  0.280,  deepest hole -0.394,  1-sigma level  0.068
Q1    1   0.4099  0.8199  0.2500  10.50000  0.05    0.28
Q2    1   0.3332  0.7970  0.1734  11.00000  0.05    0.27
Q3    1   0.2123  0.6636  0.1785  11.00000  0.05    0.26
Q4    1   0.2196  1.2236  0.3385  11.00000  0.05    0.24
Q5    1   0.2588  0.7591  0.0920  11.00000  0.05    0.23
Q6    1   0.1542  0.8605  0.1123  11.00000  0.05    0.23
Q7    1   0.1944  0.8087  0.0425  11.00000  0.05    0.22
Q8    1   0.4914  1.0945  0.1665  11.00000  0.05    0.19
Q9    1   0.3333  0.6667  0.1141  10.33333  0.05    0.19
Q10   1   0.3345  0.8592  0.0467  11.00000  0.05    0.19
Q11   1   0.3952  0.9234  0.1285  11.00000  0.05    0.19
Q12   1   0.6982  1.1240  0.1014  11.00000  0.05    0.18
Q13   1   0.3123  1.0000  0.0000  10.50000  0.05    0.18
Q14   1   0.6070  1.1821  0.0535  11.00000  0.05    0.16
Q15   1   0.6034  1.0957  0.1723  11.00000  0.05    0.16
Q16   1   0.5365  1.2005  0.2514  11.00000  0.05    0.16
Q17   1   0.0257  1.0582  0.4417  11.00000  0.05    0.16
Q18   1   0.1454  0.8864  0.0102  11.00000  0.05    0.15
Q19   1   0.4649  0.9297  0.2500  10.50000  0.05    0.15
Q20   1   0.2236  0.9732  0.0696  11.00000  0.05    0.15
;
_shelx_res_checksum              30031
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 0.333333 0.666667 0.250000 0.0240(2) Uani 1 6 d S T P
O1 O 0.3091(4) 0.8908(3) 0.1069(3) 0.0357(5) Uani 1 1 d . . .
C1 C 0.4414(6) 1.000000 0.000000 0.0397(11) Uani 1 2 d S T P
H1 H 0.570850 1.000001 0.000003 0.048 Uiso 1 2 calc R U P
N1 N 0.000000 1.000000 0.250000 0.056(2) Uani 1 6 d DS T P
H2 H 0.085(12) 1.118(7) 0.310(7) 0.068 Uiso 0.6667 1 d D U P
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
Ni1 0.0283(3) 0.0283(3) 0.0155(3) 0.000 0.000 0.01413(14)
O1 0.0417(13) 0.0383(12) 0.0295(11) 0.0120(9) 0.0101(10) 0.0219(10)
C1 0.0334(14) 0.050(3) 0.041(3) 0.022(2) 0.0112(11) 0.0249(13)
N1 0.038(2) 0.038(2) 0.093(7) 0.000 0.000 0.0191(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.2309 0.4094 '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
O1 Ni1 O1 94.63(13) 12_565 3_565
O1 Ni1 O1 91.68(9) 12_565 11
O1 Ni1 O1 82.62(12) 3_565 11
O1 Ni1 O1 82.62(12) 12_565 2_665
O1 Ni1 O1 91.68(9) 3_565 2_665
O1 Ni1 O1 171.61(13) 11 2_665
O1 Ni1 O1 171.60(13) 12_565 .
O1 Ni1 O1 91.68(9) 3_565 .
O1 Ni1 O1 94.63(13) 11 .
O1 Ni1 O1 91.68(9) 2_665 .
O1 Ni1 O1 91.68(9) 12_565 10_665
O1 Ni1 O1 171.60(13) 3_565 10_665
O1 Ni1 O1 91.68(9) 11 10_665
O1 Ni1 O1 94.63(13) 2_665 10_665
O1 Ni1 O1 82.61(12) . 10_665
C1 O1 Ni1 123.4(2) . .
O1 C1 O1 126.1(4) 8_675 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.056(2) 12_565
Ni1 O1 2.056(2) 3_565
Ni1 O1 2.056(2) 11
Ni1 O1 2.056(2) 2_665
Ni1 O1 2.056(2) .
Ni1 O1 2.056(2) 10_665
O1 C1 1.230(3) .
