#------------------------------------------------------------------------------
#$Date: 2019-11-17 15:32:33 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230902 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/14/7231404.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_7231404
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                   7.33778(19)
_cell_length_b                   7.33778(19)
_cell_length_c                   8.4822(3)
_cell_measurement_reflns_used    204
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5430
_cell_measurement_theta_min      1.8490
_cell_volume                     395.52(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         '0.10 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7
_diffrn_measured_fraction_theta_full 0.861
_diffrn_measured_fraction_theta_max 0.610
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.861
_diffrn_reflns_Laue_measured_fraction_max 0.610
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            797
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.585
_diffrn_reflns_theta_full        14.280
_diffrn_reflns_theta_max         19.928
_diffrn_reflns_theta_min         1.854
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85167
_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            colourless
_exptl_crystal_density_diffrn    1.747
_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         0.259
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 101 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.19(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         374
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0272
_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)+(0.0238P)²+0.0023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.438
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.535
_reflns_number_gt                332
_reflns_number_total             374
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cp03761b2.cif
_cod_data_source_block           AMnF_c1_p01
_cod_depositor_comments
'Adding full bibliography for 7231402--7231432.cif.'
_cod_database_code               7231404
_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_p01_s_modelR in P6(3)22
    AMnF_c1_p01_s_modelR.res
    created by SHELXL-2016/6 at 17:18:41 on 30-Mar-2017
REM P6(3)22 (#182 in standard setting)
CELL 0.41111   7.337781   7.337781   8.482206  90.0000  90.0000 120.0000
ZERR    2.00   0.000189   0.000189   0.000250   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
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
RIGU C1 O1
ACTA
L.S. 10
BOND
FMAP 2
PLAN 20
WGHT    0.023800    0.002300
FVAR       8.78782
MOLE   1
MN1   5    0.333333    0.666667    0.250000    10.16667    0.02493    0.02493 =
         0.01498    0.00000    0.00000    0.01247
N1    3    1.000000    1.000000    0.250000    10.16667    0.04040    0.04040 =
         0.16797    0.00000    0.00000    0.02020
DFIX 0.9 0.1 N1 H2
H2    2    1.083047    1.113320    0.174870    10.66667   -1.20000
O1    4    0.591919    0.894412    0.103498    11.00000    0.03453    0.03994 =
         0.03166    0.01646    0.00522    0.01721
C1    1    0.570481    1.000000    0.000000    10.50000    0.03616    0.05543 =
         0.05133    0.03154    0.01577    0.02771
AFIX  43
H1    2    0.443740    1.000000    0.000000    10.50000   -1.20000
MOLE   2
AFIX   0
HKLF 4




REM  AMnF_c1_p01_s_modelR in P6(3)22
REM R1 =  0.0272 for     332 Fo > 4sig(Fo)  and  0.0338 for all     374 data
REM     22 parameters refined using      4 restraints

END

WGHT      0.0238      0.0023

REM Highest difference peak  0.259,  deepest hole -0.360,  1-sigma level  0.066
Q1    1   0.3333  0.6667 -0.0208  10.33333  0.05    0.26
Q2    1   0.4743  0.9486  0.2500  10.50000  0.05    0.22
Q3    1   0.5824  0.9400  0.2488  11.00000  0.05    0.20
Q4    1   0.3856  0.6917  0.0731  11.00000  0.05    0.19
Q5    1   0.6239  0.8119  0.2500  10.50000  0.05    0.18
Q6    1   0.4923  0.7286  0.0316  11.00000  0.05    0.15
Q7    1   0.4593  1.0856  0.2173  11.00000  0.05    0.15
Q8    1   0.6593  0.9004  0.2148  11.00000  0.05    0.15
Q9    1   1.2987  1.1511  0.1463  11.00000  0.05    0.15
Q10   1   0.4238  0.7597  0.0139  11.00000  0.05    0.14
Q11   1   0.3500  0.9695  0.1580  11.00000  0.05    0.14
Q12   1   0.6151  0.9733  0.1651  11.00000  0.05    0.14
Q13   1   0.3219  1.0166  0.1747  11.00000  0.05    0.14
Q14   1   1.1523  1.0490  0.0633  11.00000  0.05    0.14
Q15   1   1.1053  1.2522  0.2039  11.00000  0.05    0.13
Q16   1   0.3852  0.8159  0.0170  11.00000  0.05    0.13
Q17   1   0.2998  0.9178 -0.0044  11.00000  0.05    0.13
Q18   1   1.2566  1.2244  0.1668  11.00000  0.05    0.12
Q19   1   1.0761  1.1188  0.0149  11.00000  0.05    0.12
Q20   1   0.4454  1.1748  0.0708  11.00000  0.05    0.12
;
_shelx_res_checksum              79584
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 0.0216(2) 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 1.083(11) 1.113(7) 0.175(5) 0.100 Uiso 0.6667 1 d D U P
O1 O 0.5919(2) 0.8944(3) 0.1035(2) 0.0360(4) Uani 1 1 d . . .
C1 C 0.5705(5) 1.000000 0.000000 0.0455(11) Uani 1 2 d S T P
H1 H 0.443740 1.000000 0.000000 0.055 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 0.0249(3) 0.0249(3) 0.0150(4) 0.000 0.000 0.01247(15)
N1 0.040(2) 0.040(2) 0.168(10) 0.000 0.000 0.0202(11)
O1 0.0345(9) 0.0399(9) 0.0317(11) 0.0165(7) 0.0052(7) 0.0172(8)
C1 0.0362(13) 0.055(2) 0.051(3) 0.0315(19) 0.0158(10) 0.0277(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'
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 82.35(9) 11 2_665
O1 Mn1 O1 90.80(7) 11 10_665
O1 Mn1 O1 96.96(10) 2_665 10_665
O1 Mn1 O1 90.80(7) 11 12_565
O1 Mn1 O1 169.70(8) 2_665 12_565
O1 Mn1 O1 90.80(7) 10_665 12_565
O1 Mn1 O1 169.70(8) 11 3_565
O1 Mn1 O1 90.80(7) 2_665 3_565
O1 Mn1 O1 82.35(9) 10_665 3_565
O1 Mn1 O1 96.96(10) 12_565 3_565
O1 Mn1 O1 96.96(10) 11 .
O1 Mn1 O1 90.80(7) 2_665 .
O1 Mn1 O1 169.70(8) 10_665 .
O1 Mn1 O1 82.35(9) 12_565 .
O1 Mn1 O1 90.80(7) 3_565 .
C1 O1 Mn1 123.48(18) . .
O1 C1 O1 127.5(3) . 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 2.1832(16) 11
Mn1 O1 2.1832(16) 2_665
Mn1 O1 2.1832(16) 10_665
Mn1 O1 2.1832(16) 12_565
Mn1 O1 2.1832(16) 3_565
Mn1 O1 2.1832(16) .
O1 C1 1.232(2) .
