#------------------------------------------------------------------------------
#$Date: 2019-11-17 15:32:33 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230902 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/14/7231424.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_7231424
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                   7.27890(18)
_cell_length_b                   7.27890(18)
_cell_length_c                   8.0555(2)
_cell_measurement_reflns_used    363
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.3520
_cell_measurement_theta_min      1.8690
_cell_volume                     369.619(16)
_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         '0.12 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.728
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.728
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1076
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.674
_diffrn_reflns_theta_full        14.286
_diffrn_reflns_theta_max         20.017
_diffrn_reflns_theta_min         1.869
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85616
_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    1.903
_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         0.307
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 100 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         406
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0249
_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)+(0.0159P)²+0.1083P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.390
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.567
_reflns_number_gt                373
_reflns_number_total             406
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cp03761b2.cif
_cod_data_source_block           ANiF_c2_p01
_cod_depositor_comments
'Adding full bibliography for 7231402--7231432.cif.'
_cod_original_cell_volume        369.62(2)
_cod_database_code               7231424
_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_p01_s in P6(3)22
    ANiF_c2_p01_s.res
    created by SHELXL-2016/6 at 13:08:28 on 06-Aug-2018
REM P6(3)22 (#182 in standard setting)
CELL 0.41128   7.278900   7.278900   8.055466  90.0000  90.0000 120.0000
ZERR    2.00   0.000183   0.000183   0.000238   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 -3 10 4
OMIT 0 1 1
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
ACTA
BOND
FMAP 2
PLAN 20
WGHT    0.015900    0.108300
FVAR       8.83363
MOLE   1
NI1   5    0.333333    0.666667    0.250000    10.16667    0.02205    0.02205 =
         0.01374    0.00000    0.00000    0.01103

O1    4    0.309218    0.888717    0.105971    11.00000    0.03457    0.03142 =
         0.02569    0.01051    0.00842    0.01785
C1    1    0.441270    1.000000    0.000000    10.50000    0.02833    0.03829 =
         0.03805    0.01777    0.00889    0.01915
AFIX  43
H1    2    0.569037    1.000001    0.000001    10.50000   -1.20000
MOLE   2
AFIX   0
N1    3    0.000000    1.000000    0.250000    10.16667    0.03925    0.03925 =
         0.10594    0.00000    0.00000    0.01962
DFIX 0.9 0.1 N1 H2
H2    2    0.093998    1.122668    0.314267    10.66667   -1.20000
HKLF 4




REM  ANiF_c2_p01_s in P6(3)22
REM R1 =  0.0249 for     373 Fo > 4sig(Fo)  and  0.0296 for all     406 data
REM     22 parameters refined using      0 restraints

END

WGHT      0.0162      0.1078

REM Highest difference peak  0.307,  deepest hole -0.256,  1-sigma level  0.060
Q1    1   0.2823  0.7454 -0.0054  11.00000  0.05    0.21
Q2    1   0.3816  0.7594  0.0670  11.00000  0.05    0.21
Q3    1   0.0928  1.0928  0.5000  10.50000  0.05    0.20
Q4    1   0.2646  0.8356  0.0527  11.00000  0.05    0.20
Q5    1   0.7073  1.1296  0.1039  11.00000  0.05    0.19
Q6    1   0.1614  0.8877  0.0322  11.00000  0.05    0.18
Q7    1   0.3079  1.0000  0.0000  10.50000  0.05    0.17
Q8    1   0.3799  0.9921  0.1817  11.00000  0.05    0.17
Q9    1   0.2699  1.2964  0.2522  11.00000  0.05    0.17
Q10   1   0.2684  0.9586  0.0950  11.00000  0.05    0.16
Q11   1   0.0448  1.0781  0.3689  11.00000  0.05    0.16
Q12   1   0.3284  0.7972  0.0832  11.00000  0.05    0.16
Q13   1   0.3780  0.8251  0.1700  11.00000  0.05    0.15
Q14   1   0.2855  0.7822  0.1610  11.00000  0.05    0.15
Q15   1   0.2027  0.7973  0.2500  10.50000  0.05    0.15
Q16   1   0.1750  0.8861 -0.0460  11.00000  0.05    0.14
Q17   1   0.1317  1.1172  0.3737  11.00000  0.05    0.14
Q18   1   0.3648  0.8898  0.2517  11.00000  0.05    0.14
Q19   1   0.2494  1.2559  0.3363  11.00000  0.05    0.14
Q20   1   0.5407  0.8640  0.1035  11.00000  0.05    0.14
;
_shelx_res_checksum              84151
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 0.0193(2) Uani 1 6 d S T P
O1 O 0.3092(3) 0.8887(3) 0.1060(2) 0.0300(4) Uani 1 1 d . . .
C1 C 0.4413(5) 1.000000 0.000000 0.0338(8) Uani 1 2 d S T P
H1 H 0.569037 1.000001 0.000001 0.041 Uiso 1 2 calc R U P
N1 N 0.000000 1.000000 0.250000 0.061(2) Uani 1 6 d DS T P
H2 H 0.094(10) 1.123(7) 0.314(6) 0.074 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 0.0221(2) 0.0221(2) 0.0137(3) 0.000 0.000 0.01103(12)
O1 0.0346(10) 0.0314(9) 0.0257(10) 0.0105(7) 0.0084(7) 0.0179(8)
C1 0.0283(12) 0.0383(19) 0.038(2) 0.0178(17) 0.0089(8) 0.0191(9)
N1 0.039(2) 0.039(2) 0.106(7) 0.000 0.000 0.0196(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 91.57(7) 10_665 11
O1 Ni1 O1 94.76(11) 10_665 2_665
O1 Ni1 O1 171.57(10) 11 2_665
O1 Ni1 O1 171.57(10) 10_665 3_565
O1 Ni1 O1 82.70(10) 11 3_565
O1 Ni1 O1 91.57(7) 2_665 3_565
O1 Ni1 O1 91.57(7) 10_665 12_565
O1 Ni1 O1 91.57(7) 11 12_565
O1 Ni1 O1 82.70(10) 2_665 12_565
O1 Ni1 O1 94.76(11) 3_565 12_565
O1 Ni1 O1 82.70(10) 10_665 .
O1 Ni1 O1 94.76(11) 11 .
O1 Ni1 O1 91.57(7) 2_665 .
O1 Ni1 O1 91.57(7) 3_565 .
O1 Ni1 O1 171.57(10) 12_565 .
C1 O1 Ni1 123.87(19) . .
O1 C1 O1 126.6(3) . 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 2.0671(17) 10_665
Ni1 O1 2.0671(17) 11
Ni1 O1 2.0671(17) 2_665
Ni1 O1 2.0671(17) 3_565
Ni1 O1 2.0671(17) 12_565
Ni1 O1 2.0671(17) .
O1 C1 1.237(2) .
