#------------------------------------------------------------------------------
#$Date: 2019-11-17 15:32:33 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230902 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/14/7231421.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_7231421
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 Fe O6, N H4'
_chemical_formula_sum            'C3 H7 Fe N O6'
_chemical_formula_weight         208.95
_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                   7.30440(13)
_cell_length_b                   7.30440(13)
_cell_length_c                   8.31833(18)
_cell_measurement_reflns_used    221
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.4310
_cell_measurement_theta_min      1.8620
_cell_volume                     384.358(13)
_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         '0.19 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.565
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41111
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.867
_diffrn_reflns_Laue_measured_fraction_max 0.565
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            782
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.547
_diffrn_reflns_theta_full        14.280
_diffrn_reflns_theta_max         20.320
_diffrn_reflns_theta_min         1.862
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  1.141
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_description       block
_exptl_crystal_F_000             212
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 96 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         363
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.255
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0262
_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)+(0.0234P)²+0.0033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.464
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.511
_reflns_number_gt                319
_reflns_number_total             363
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cp03761b2.cif
_cod_data_source_block           AFeF_c4_p02
_cod_depositor_comments
'Adding full bibliography for 7231402--7231432.cif.'
_cod_original_cell_volume        384.358(16)
_cod_database_code               7231421
_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 AFeF_c4_p02_s in P6(3)22
    AFeF_c4_p02_s.res
    created by SHELXL-2016/6 at 18:20:17 on 25-Apr-2017
REM P6(3)22 (#182 in standard setting)
CELL 0.41111   7.304404   7.304404   8.318334  90.0000  90.0000 120.0000
ZERR    2.00   0.000126   0.000126   0.000183   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 Fe
DISP $C -0.00006  0.00048  5.14124!source kissel
DISP $H -0.00003  0.00000  0.64128!source kissel
DISP $N  0.00062  0.00099  7.19094!source kissel
DISP $O  0.00180  0.00183 10.15590!source kissel
DISP $Fe  0.19668  0.30563 740.81318!source kissel
UNIT 6.00 14.00 2.00 12.00 2.00
LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
ACTA
L.S. 10
BOND
FMAP 2
PLAN 20
DELU C1 O1

WGHT    0.023400    0.003300
FVAR       7.84798
MOLE   1
FE1   5    0.333333    0.666667    0.250000    10.16667    0.02454    0.02454 =
         0.01292    0.00000    0.00000    0.01227
N1    3    1.000000    1.000000    0.250000    10.16667    0.03810    0.03810 =
         0.12563    0.00000    0.00000    0.01905
DFIX  0.9 0.1 N1 H2
H2    2    1.087397    1.116116    0.177066    10.66667   -1.20000
O1    4    0.587078    0.891932    0.104898    11.00000    0.03392    0.03536 =
         0.02868    0.01287    0.00364    0.01581
C1    1    0.564919    1.000000    0.000000    10.50000    0.03184    0.04613 =
         0.04423    0.02361    0.01180    0.02306
AFIX  43
H1    2    0.437598    0.999998   -0.000001    10.50000   -1.20000
MOLE   2
AFIX   0
HKLF 4




REM  AFeF_c4_p02_s in P6(3)22
REM R1 =  0.0262 for     319 Fo > 4sig(Fo)  and  0.0335 for all     363 data
REM     22 parameters refined using      2 restraints

END

WGHT      0.0235      0.0033

REM Highest difference peak  0.226,  deepest hole -0.315,  1-sigma level  0.069
Q1    1   0.4329  1.1323  0.0911  11.00000  0.05    0.23
Q2    1   1.1078  1.1824 -0.0048  11.00000  0.05    0.19
Q3    1   0.5912  1.2956  0.2500  10.50000  0.05    0.18
Q4    1   0.9360  0.8720  0.2500  10.50000  0.05    0.17
Q5    1   0.5035  1.1734  0.1568  11.00000  0.05    0.17
Q6    1   1.0679  1.1359  0.2500  10.50000  0.05    0.16
Q7    1   0.4562  1.1155  0.2170  11.00000  0.05    0.16
Q8    1   0.5826  0.9454  0.0881  11.00000  0.05    0.15
Q9    1   0.5269  0.9726  0.2487  11.00000  0.05    0.15
Q10   1   0.6807  1.2181  0.2491  11.00000  0.05    0.15
Q11   1   0.6667  1.3333  0.1591  10.33333  0.05    0.15
Q12   1   0.2954  0.9161  0.0024  11.00000  0.05    0.14
Q13   1   0.2059  1.0000  0.0000  10.50000  0.05    0.14
Q14   1   0.6762  0.9940  0.2216  11.00000  0.05    0.14
Q15   1   1.0785  1.0251  0.0760  11.00000  0.05    0.14
Q16   1   0.5440  1.2703  0.1712  11.00000  0.05    0.13
Q17   1   0.6400  1.0531  0.1730  11.00000  0.05    0.13
Q18   1   0.4715  1.1243 -0.0030  11.00000  0.05    0.13
Q19   1   0.9510  1.2617  0.1834  11.00000  0.05    0.13
Q20   1   0.5124  1.0905  0.0835  11.00000  0.05    0.13
;
_shelx_res_checksum              70380
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
Fe1 Fe 0.333333 0.666667 0.250000 0.0207(3) Uani 1 6 d S T P
N1 N 1.000000 1.000000 0.250000 0.067(2) Uani 1 6 d DS T P
H2 H 1.087(11) 1.116(7) 0.177(4) 0.081 Uiso 0.6667 1 d D U P
O1 O 0.5871(3) 0.8919(3) 0.1049(3) 0.0333(5) Uani 1 1 d . U .
C1 C 0.5649(6) 1.000000 0.000000 0.0391(11) Uani 1 2 d S TU P
H1 H 0.437598 0.999998 -0.000001 0.047 Uiso 1 2 calc R 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
Fe1 0.0245(3) 0.0245(3) 0.0129(5) 0.000 0.000 0.01227(16)
N1 0.038(2) 0.038(2) 0.126(8) 0.000 0.000 0.0190(12)
O1 0.0339(10) 0.0354(11) 0.0287(13) 0.0129(8) 0.0036(8) 0.0158(9)
C1 0.0318(15) 0.046(3) 0.044(3) 0.024(2) 0.0118(10) 0.0231(13)
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'
Fe Fe 0.1967 0.3056 '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 Fe1 O1 82.38(10) 11 2_665
O1 Fe1 O1 91.13(8) 11 10_665
O1 Fe1 O1 96.17(12) 2_665 10_665
O1 Fe1 O1 170.31(11) 11 3_565
O1 Fe1 O1 91.13(8) 2_665 3_565
O1 Fe1 O1 82.38(10) 10_665 3_565
O1 Fe1 O1 91.13(8) 11 12_565
O1 Fe1 O1 170.31(11) 2_665 12_565
O1 Fe1 O1 91.13(8) 10_665 12_565
O1 Fe1 O1 96.17(12) 3_565 12_565
O1 Fe1 O1 96.17(12) 11 .
O1 Fe1 O1 91.13(8) 2_665 .
O1 Fe1 O1 170.31(11) 10_665 .
O1 Fe1 O1 91.13(8) 3_565 .
O1 Fe1 O1 82.38(10) 12_565 .
C1 O1 Fe1 123.3(2) . .
O1 C1 O1 126.7(4) . 8_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.1330(19) 11
Fe1 O1 2.1330(19) 2_665
Fe1 O1 2.1330(19) 10_665
Fe1 O1 2.1330(19) 3_565
Fe1 O1 2.1330(19) 12_565
Fe1 O1 2.1330(19) .
O1 C1 1.240(3) .
