#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:32:33 +0100 (dom 17 de nov de 2019) $
#$Revision: 230902 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/14/7231403.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_7231403
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 Mn O6, N H4'
_chemical_formula_sum            'C3 H7 Mn N O6'
_chemical_formula_weight         208.04
_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                   7.32804(14)
_cell_length_b                   7.32804(14)
_cell_length_c                   8.49640(19)
_cell_measurement_reflns_used    220
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.1390
_cell_measurement_theta_min      1.8550
_cell_volume                     395.131(14)
_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         '0.25 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7
_diffrn_measured_fraction_theta_full 0.850
_diffrn_measured_fraction_theta_max 0.657
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.850
_diffrn_reflns_Laue_measured_fraction_max 0.657
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            804
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.633
_diffrn_reflns_theta_full        14.280
_diffrn_reflns_theta_max         19.337
_diffrn_reflns_theta_min         1.856
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86549
_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    1.749
_exptl_crystal_description       block
_exptl_crystal_F_000             210
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.073
_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   -0.01(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         371
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0301
_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)+(0.0223P)²+0.0626P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.444
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.585
_reflns_number_gt                333
_reflns_number_total             371
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cp03761b2.cif
_cod_data_source_block           AMnF_c1_p02
_cod_depositor_comments
'Adding full bibliography for 7231402--7231432.cif.'
_cod_original_cell_volume        395.131(18)
_cod_database_code               7231403
_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 AMnF_c1_p02_s_modelR in P6(3)22
    AMnF_c1_p02_s_modelR.res
    created by SHELXL-2016/6 at 17:24:04 on 30-Mar-2017
REM P6(3)22 (#182 in standard setting)
CELL 0.41111   7.328045   7.328045   8.496400  90.0000  90.0000 120.0000
ZERR    2.00   0.000145   0.000145   0.000194   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 Mn
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Mn  0.17888  0.26125 635.04629!source kissel
UNIT 6.00 14.00 2.00 12.00 2.00
OMIT -1 2 0
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
RIGU C1 O1
ACTA
L.S. 10
BOND
FMAP 2
PLAN 20
WGHT    0.022300    0.062600
FVAR       9.04685
MOLE   1
MN1   5    0.333333    0.666667    0.250000    10.16667    0.02700    0.02700 =
         0.01578    0.00000    0.00000    0.01350
N1    3    1.000000    1.000000    0.250000    10.16667    0.03956    0.03956 =
         0.17019    0.00000    0.00000    0.01978
DFIX 0.9 0.05 N1 H2
H2    2    1.085347    1.110869    0.174660    10.66667   -1.20000
O1    4    0.592184    0.894549    0.103872    11.00000    0.03727    0.04195 =
         0.03408    0.01653    0.00599    0.01805
C1    1    0.570345    1.000000    0.000000    10.50000    0.03824    0.06395 =
         0.05304    0.03362    0.01681    0.03198
AFIX  43
H1    2    0.443435    0.999999    0.000001    10.50000   -1.20000
MOLE   2
AFIX   0
HKLF 4




REM  AMnF_c1_p02_s_modelR in P6(3)22
REM R1 =  0.0301 for     333 Fo > 4sig(Fo)  and  0.0359 for all     371 data
REM     22 parameters refined using      4 restraints

END

WGHT      0.0223      0.0626

REM Highest difference peak  0.289,  deepest hole -0.323,  1-sigma level  0.073
Q1    1   0.5841  1.1681  0.2500  10.50000  0.05    0.29
Q2    1   0.3333  0.6667  0.0040  10.33333  0.05    0.27
Q3    1   0.6667  1.3333  0.2145  10.33333  0.05    0.25
Q4    1   0.4235  1.1661  0.1116  11.00000  0.05    0.22
Q5    1   0.5139  1.1641  0.0492  11.00000  0.05    0.19
Q6    1   0.5493  1.1195  0.1483  11.00000  0.05    0.18
Q7    1   0.4929  1.2244  0.1604  11.00000  0.05    0.18
Q8    1   0.4954  1.2147  0.0552  11.00000  0.05    0.18
Q9    1   0.4787  1.1879  0.2300  11.00000  0.05    0.17
Q10   1   0.9393  0.8785  0.2500  10.50000  0.05    0.16
Q11   1   1.2974  1.1494  0.1311  11.00000  0.05    0.15
Q12   1   1.0665  1.1353  0.0157  11.00000  0.05    0.15
Q13   1   1.0000  1.0000  0.0000  10.16667  0.05    0.15
Q14   1   1.3431  1.1763  0.1991  11.00000  0.05    0.15
Q15   1   0.4989  1.0014  0.2043  11.00000  0.05    0.14
Q16   1   1.0556  1.1112  0.2500  10.50000  0.05    0.12
Q17   1   0.5852  0.9885  0.2762  11.00000  0.05    0.12
Q18   1   0.7813  1.1001  0.1172  11.00000  0.05    0.11
Q19   1   0.4179  0.7093  0.0595  11.00000  0.05    0.11
Q20   1   0.6462  1.0782  0.2677  11.00000  0.05    0.11
;
_shelx_res_checksum              79977
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
Mn1 Mn 0.333333 0.666667 0.250000 0.0233(3) Uani 1 6 d S T P
N1 N 1.000000 1.000000 0.250000 0.083(3) Uani 1 6 d DS T P
H2 H 1.085(13) 1.111(8) 0.175(6) 0.100 Uiso 0.6667 1 d D U P
O1 O 0.5922(3) 0.8945(3) 0.1039(3) 0.0385(6) Uani 1 1 d . . .
C1 C 0.5703(6) 1.000000 0.000000 0.0489(13) Uani 1 2 d S T P
H1 H 0.443435 0.999999 0.000001 0.059 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
Mn1 0.0270(4) 0.0270(4) 0.0158(5) 0.000 0.000 0.01350(18)
N1 0.040(3) 0.040(3) 0.170(12) 0.000 0.000 0.0198(13)
O1 0.0373(11) 0.0419(12) 0.0341(15) 0.0165(9) 0.0060(9) 0.0181(10)
C1 0.0382(16) 0.064(3) 0.053(3) 0.034(2) 0.0168(12) 0.0320(15)
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'
Mn Mn 0.1789 0.2612 '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 Mn1 O1 82.32(11) 11 2_665
O1 Mn1 O1 90.82(9) 11 10_665
O1 Mn1 O1 96.97(12) 2_665 10_665
O1 Mn1 O1 96.97(12) 11 .
O1 Mn1 O1 90.82(9) 2_665 .
O1 Mn1 O1 169.66(10) 10_665 .
O1 Mn1 O1 90.82(9) 11 12_565
O1 Mn1 O1 169.67(10) 2_665 12_565
O1 Mn1 O1 90.82(9) 10_665 12_565
O1 Mn1 O1 82.32(11) . 12_565
O1 Mn1 O1 169.67(10) 11 3_565
O1 Mn1 O1 90.82(9) 2_665 3_565
O1 Mn1 O1 82.31(11) 10_665 3_565
O1 Mn1 O1 90.82(9) . 3_565
O1 Mn1 O1 96.97(12) 12_565 3_565
C1 O1 Mn1 123.4(2) . .
O1 C1 O1 127.5(4) . 8_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.182(2) 11
Mn1 O1 2.182(2) 2_665
Mn1 O1 2.182(2) 10_665
Mn1 O1 2.182(2) .
Mn1 O1 2.182(2) 12_565
Mn1 O1 2.182(2) 3_565
O1 C1 1.235(3) .
