#------------------------------------------------------------------------------
#$Date: 2019-11-17 15:32:33 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230902 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/14/7231420.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_7231420
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                   7.2211(2)
_cell_length_b                   7.2211(2)
_cell_length_c                   8.0490(3)
_cell_measurement_reflns_used    393
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.8030
_cell_measurement_theta_min      1.8840
_cell_volume                     363.48(2)
_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         '0.51 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  0.0324
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.728
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1063
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.667
_diffrn_reflns_theta_full        14.286
_diffrn_reflns_theta_max         20.083
_diffrn_reflns_theta_min         1.884
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38672
_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    1.935
_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         0.590
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 98 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         400
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0298
_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)+(0.0071P)²+0.2148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.378
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.547
_reflns_number_gt                370
_reflns_number_total             401
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cp03761b2.cif
_cod_data_source_block           ANiF_c2_p03
_cod_depositor_comments
'Adding full bibliography for 7231402--7231432.cif.'
_cod_database_code               7231420
_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_p03_s in P6(3)22
    ANiF_c2_p03_s.res
    created by SHELXL-2016/6 at 14:09:38 on 06-Aug-2018
REM P6(3)22 (#182 in standard setting)
CELL 0.41128   7.221081   7.221081   8.048978  90.0000  90.0000 120.0000
ZERR    2.00   0.000207   0.000207   0.000268   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 0 4 12 !High (Fobs-Fcalc)/sigma
OMIT 0 1 1
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
ACTA
BOND
FMAP 2
PLAN 20
WGHT    0.007100    0.214800
FVAR       8.91566
MOLE   1
NI1   5    0.333333    0.666667    0.250000    10.16667    0.02153    0.02153 =
         0.01223    0.00000    0.00000    0.01076
O1    4    0.308886    0.889366    0.106699    11.00000    0.03436    0.03130 =
         0.02587    0.01117    0.00880    0.01774
C1    1    0.441484    1.000000    0.000000    10.50000    0.02815    0.04079 =
         0.03984    0.02017    0.01009    0.02040
AFIX  43
H1    2    0.570273    1.000000   -0.000001    10.50000   -1.20000
MOLE   2
REM #####
AFIX   0
N1    3    0.000000    1.000000    0.250000    10.16667    0.03682    0.03682 =
         0.09843    0.00000    0.00000    0.01841
DFIX 0.9 0.1 N1 H2
H2    2    0.089998    1.119001    0.314400    10.66667   -1.20000
HKLF 4




REM  ANiF_c2_p03_s in P6(3)22
REM R1 =  0.0298 for     369 Fo > 4sig(Fo)  and  0.0333 for all     400 data
REM     22 parameters refined using      0 restraints

END

WGHT      0.0071      0.2148

REM Highest difference peak  0.590,  deepest hole -0.454,  1-sigma level  0.085
Q1    1  -0.0513  0.8975  0.2500  10.50000  0.05    0.59
Q2    1   0.2701  0.5401  0.2500  10.50000  0.05    0.59
Q3    1   0.3988  0.7975  0.2500  10.50000  0.05    0.55
Q4    1   0.0572  1.1145  0.2500  10.50000  0.05    0.40
Q5    1   0.3324  0.7964  0.1633  11.00000  0.05    0.33
Q6    1   0.4552  0.9104  0.2500  10.50000  0.05    0.29
Q7    1   0.2074  0.6607  0.1910  11.00000  0.05    0.28
Q8    1   0.2695  0.7801  0.1361  11.00000  0.05    0.27
Q9    1   0.1411  0.8647 -0.0104  11.00000  0.05    0.27
Q10   1   0.3977  0.9556  0.1341  11.00000  0.05    0.26
Q11   1   0.3144  0.9463  0.0116  11.00000  0.05    0.26
Q12   1   0.2034  0.8508  0.0485  11.00000  0.05    0.26
Q13   1   0.4386  1.0377  0.0557  11.00000  0.05    0.24
Q14   1   0.1997  0.9411  0.0991  11.00000  0.05    0.24
Q15   1   0.1946  1.1007  0.4198  11.00000  0.05    0.23
Q16   1   0.3366  0.8597  0.0522  11.00000  0.05    0.23
Q17   1   0.6579  1.2418  0.2240  11.00000  0.05    0.22
Q18   1   0.5192  1.2547  0.1830  11.00000  0.05    0.21
Q19   1  -0.0046  1.1405  0.3719  11.00000  0.05    0.21
Q20   1   0.2664  1.0187  0.0501  11.00000  0.05    0.20
;
_shelx_res_checksum              62739
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 0.0184(2) Uani 1 6 d S T P
O1 O 0.3089(3) 0.8894(3) 0.1067(3) 0.0299(5) Uani 1 1 d . . .
C1 C 0.4415(5) 1.000000 0.000000 0.0349(10) Uani 1 2 d S T P
H1 H 0.570273 1.000000 -0.000001 0.042 Uiso 1 2 calc R U P
N1 N 0.000000 1.000000 0.250000 0.057(2) Uani 1 6 d DS T P
H2 H 0.090(11) 1.119(7) 0.314(7) 0.069 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 0.0215(3) 0.0215(3) 0.0122(3) 0.000 0.000 0.01076(13)
O1 0.0344(11) 0.0313(10) 0.0259(11) 0.0112(8) 0.0088(9) 0.0177(9)
C1 0.0281(14) 0.041(2) 0.040(3) 0.020(2) 0.0101(10) 0.0204(11)
N1 0.037(2) 0.037(2) 0.098(7) 0.000 0.000 0.0184(11)
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 82.59(11) . 10_665
O1 Ni1 O1 91.63(8) . 2_665
O1 Ni1 O1 94.78(12) 10_665 2_665
O1 Ni1 O1 94.78(12) . 11
O1 Ni1 O1 91.63(8) 10_665 11
O1 Ni1 O1 171.47(12) 2_665 11
O1 Ni1 O1 91.63(8) . 3_565
O1 Ni1 O1 171.47(12) 10_665 3_565
O1 Ni1 O1 91.63(8) 2_665 3_565
O1 Ni1 O1 82.59(11) 11 3_565
O1 Ni1 O1 171.48(12) . 12_565
O1 Ni1 O1 91.63(8) 10_665 12_565
O1 Ni1 O1 82.59(11) 2_665 12_565
O1 Ni1 O1 91.63(8) 11 12_565
O1 Ni1 O1 94.78(12) 3_565 12_565
C1 O1 Ni1 123.6(2) . .
O1 C1 O1 126.3(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 2.0571(19) .
Ni1 O1 2.0571(19) 10_665
Ni1 O1 2.0571(19) 2_665
Ni1 O1 2.0571(19) 11
Ni1 O1 2.0571(19) 3_565
Ni1 O1 2.0571(19) 12_565
O1 C1 1.236(3) .
