#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:32:33 +0100 (dom 17 de nov de 2019) $
#$Revision: 230902 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/14/7231413.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_7231413
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                   7.31630(11)
_cell_length_b                   7.31630(11)
_cell_length_c                   8.31849(16)
_cell_measurement_reflns_used    237
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.4140
_cell_measurement_theta_min      1.8620
_cell_volume                     385.619(11)
_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 0.861
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.861
_diffrn_reflns_Laue_measured_fraction_max 0.565
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            785
_diffrn_reflns_point_group_measured_fraction_full 0.896
_diffrn_reflns_point_group_measured_fraction_max 0.548
_diffrn_reflns_theta_full        14.280
_diffrn_reflns_theta_max         20.287
_diffrn_reflns_theta_min         1.859
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.800
_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         0.260
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.065
_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   0.21(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         364
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0277
_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)+(0.0218P)²+0.1299P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.468
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.516
_reflns_number_gt                320
_reflns_number_total             364
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cp03761b2.cif
_cod_data_source_block           AFeF_c4_p01
_cod_depositor_comments
'Adding full bibliography for 7231402--7231432.cif.'
_cod_original_cell_volume        385.618(14)
_cod_database_code               7231413
_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_p01_s in P6(3)22
    AFeF_c4_p01_s.res
    created by SHELXL-2016/6 at 13:56:02 on 23-May-2017
REM P6(3)22 (#182 in standard setting)
CELL 0.41111   7.316297   7.316297   8.318487  90.0000  90.0000 120.0000
ZERR    2.00   0.000113   0.000113   0.000158   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
OMIT -1 2 2
OMIT 0 1 1
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!

ACTA
L.S. 10
BOND
FMAP 2
PLAN 20
DELU C1 O1

WGHT    0.021800    0.129900
FVAR       7.96612
MOLE   1
FE1   5    0.333333    0.666667    0.250000    10.16667    0.02392    0.02392 =
         0.01320    0.00000    0.00000    0.01196
N1    3    1.000000    1.000000    0.250000    10.16667    0.03678    0.03678 =
         0.12596    0.00000    0.00000    0.01839
DFIX  0.9 0.1 N1 H2
H2    2    1.099488    1.127246    0.180145    10.66667   -1.20000
O1    4    0.586798    0.891872    0.104553    11.00000    0.03406    0.03654 =
         0.02774    0.01232    0.00257    0.01674
C1    1    0.564864    1.000000    0.000000    10.50000    0.02981    0.04404 =
         0.04638    0.02594    0.01297    0.02202
AFIX  43
H1    2    0.437749    0.999997    0.000000    10.50000   -1.20000
MOLE   2
AFIX   0
HKLF 4




REM  AFeF_c4_p01_s in P6(3)22
REM R1 =  0.0277 for     320 Fo > 4sig(Fo)  and  0.0354 for all     364 data
REM     22 parameters refined using      2 restraints

END

WGHT      0.0218      0.1315

REM Highest difference peak  0.260,  deepest hole -0.273,  1-sigma level  0.065
Q1    1   0.3331  1.0270  0.0578  11.00000  0.05    0.26
Q2    1   0.9394  0.8789  0.2500  10.50000  0.05    0.25
Q3    1   0.6907  0.9993  0.2364  11.00000  0.05    0.22
Q4    1   0.6658  1.0000  0.0000  10.50000  0.05    0.22
Q5    1   0.4094  1.0741  0.1060  11.00000  0.05    0.21
Q6    1   0.4192  0.8157  0.1462  11.00000  0.05    0.20
Q7    1   1.0838  1.1316 -0.0042  11.00000  0.05    0.20
Q8    1   0.6732  0.8078  0.0000  11.00000  0.05    0.18
Q9    1   0.6263  0.9914  0.1055  11.00000  0.05    0.17
Q10   1   0.4600  0.7232  0.0927  11.00000  0.05    0.17
Q11   1   0.3269  0.9046  0.1101  11.00000  0.05    0.16
Q12   1   0.3013  0.9118 -0.0012  11.00000  0.05    0.16
Q13   1   1.0575  1.2772  0.1225  11.00000  0.05    0.15
Q14   1   1.1375  1.2750  0.2500  10.50000  0.05    0.15
Q15   1   0.4921  1.1046  0.0523  11.00000  0.05    0.15
Q16   1   1.1280  1.1255  0.1309  11.00000  0.05    0.15
Q17   1   0.7417  1.2102  0.1074  11.00000  0.05    0.15
Q18   1   0.6646  0.8646  0.1667  11.00000  0.05    0.14
Q19   1   0.5243  1.1617  0.1566  11.00000  0.05    0.14
Q20   1   0.2215  1.0000  0.0000  10.50000  0.05    0.14
;
_shelx_res_checksum              36297
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 0.0203(3) Uani 1 6 d S T P
N1 N 1.000000 1.000000 0.250000 0.067(3) Uani 1 6 d DS T P
H2 H 1.099(12) 1.127(8) 0.180(6) 0.080 Uiso 0.6667 1 d D U P
O1 O 0.5868(4) 0.8919(4) 0.1046(3) 0.0332(6) Uani 1 1 d . U .
C1 C 0.5649(6) 1.000000 0.000000 0.0385(13) Uani 1 2 d S TU P
H1 H 0.437749 0.999997 0.000000 0.046 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 0.0239(4) 0.0239(4) 0.0132(5) 0.000 0.000 0.01196(18)
N1 0.037(3) 0.037(3) 0.126(9) 0.000 0.000 0.0184(13)
O1 0.0341(12) 0.0365(13) 0.0277(14) 0.0123(10) 0.0026(10) 0.0167(11)
C1 0.0298(16) 0.044(3) 0.046(4) 0.026(2) 0.0130(12) 0.0220(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 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 82.49(12) 11 2_665
O1 Fe1 O1 91.07(10) 11 10_665
O1 Fe1 O1 96.16(14) 2_665 10_665
O1 Fe1 O1 96.16(14) 11 .
O1 Fe1 O1 91.07(10) 2_665 .
O1 Fe1 O1 170.38(12) 10_665 .
O1 Fe1 O1 170.38(12) 11 3_565
O1 Fe1 O1 91.07(10) 2_665 3_565
O1 Fe1 O1 82.49(12) 10_665 3_565
O1 Fe1 O1 91.07(10) . 3_565
O1 Fe1 O1 91.07(10) 11 12_565
O1 Fe1 O1 170.38(12) 2_665 12_565
O1 Fe1 O1 91.07(10) 10_665 12_565
O1 Fe1 O1 82.49(12) . 12_565
O1 Fe1 O1 96.16(14) 3_565 12_565
C1 O1 Fe1 123.4(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 2.136(2) 11
Fe1 O1 2.136(2) 2_665
Fe1 O1 2.136(2) 10_665
Fe1 O1 2.136(2) .
Fe1 O1 2.136(2) 3_565
Fe1 O1 2.136(2) 12_565
O1 C1 1.239(3) .
