#------------------------------------------------------------------------------
#$Date: 2017-01-09 05:02:49 +0200 (Mon, 09 Jan 2017) $
#$Revision: 190064 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/68/7226832.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_7226832
loop_
_publ_author_name
'Collings, Ines E.'
'Bykov, Maxim'
'Bykova, Elena'
'Tucker, Matthew G.'
'Petitgirard, Sylvain'
'Hanfland, Michael'
'Glazyrin, Konstantin'
'van Smaalen, Sander'
'Goodwin, Andrew L.'
'Dubrovinsky, Leonid'
'Dubrovinskaia, Natalia'
_publ_section_title
;
 Structural distortions in the high-pressure polar phases of ammonium
 metal formates
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8849
_journal_paper_doi               10.1039/C6CE01891B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C3 H7 N Ni O6'
_chemical_formula_weight         211.81
_chemical_name_systematic        'ammonium nickel formate'
_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-2014
_audit_update_record
;
2016-08-29 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   7.1208(6)
_cell_length_b                   7.1208(6)
_cell_length_c                   8.0513(4)
_cell_measurement_reflns_used    468
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.1110
_cell_measurement_theta_min      3.6260
_cell_volume                     353.55(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX (Sheldrick, 2007)'
_diffrn_ambient_pressure         'at 1.28 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.706
_diffrn_measurement_device_type  'ID09A beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41168
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.706
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1156
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.638
_diffrn_reflns_theta_full        14.301
_diffrn_reflns_theta_max         21.096
_diffrn_reflns_theta_min         2.931
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48868
_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            green
_exptl_crystal_density_diffrn    1.990
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 74 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.22(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         430
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0496
_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)+(0.0430P)²+0.4766P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.369
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.507
_reflns_number_gt                334
_reflns_number_total             430
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01891b2.cif
_cod_data_source_block           ANiF_p02
_cod_depositor_comments
'Adding full bibliography for 7226831--7226836.cif.'
_cod_original_cell_volume        353.56(6)
_cod_database_code               7226832
_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.
;
_shelxl_version_number           2014-3
_shelx_res_file
;
TITL nh4fe_c4_p02_s_test4 in P6(3)22
REM P6(3)22 (#182 in standard setting)
CELL 0.41168   7.120827   7.120827   8.051324  90.0000  90.0000 120.0000
ZERR    2.00   0.000582   0.000582   0.000370   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 NI C H O N
DISP $Ni  0.23122  0.41013 990.48791!source kissel
DISP $C -0.00005  0.00048  5.14755!source kissel
DISP $H -0.00003  0.00000  0.64142!source kissel
DISP $O  0.00181  0.00183 10.17764!source kissel
DISP $N  0.00063  0.00099  7.20319!source kissel
UNIT 2.000 6 14 12 2.000
OMIT 0 1 1

ACTA
LIST 4

L.S. 20
BOND
FMAP 2
PLAN 20

EQIV $1 1-y, -1+x-y, +z
RIGU C1 O1

WGHT    0.043000    0.476600
FVAR      10.91469
NI1   1    0.666667    0.333333    0.250000    10.16667    0.04345    0.04345 =
         0.01897    0.00000    0.00000    0.02172
O1    4    0.691605    0.108363    0.107945    11.00000    0.05989    0.05610 =
         0.03341   -0.01536   -0.01376    0.03205
N1    5    1.000000    0.000000    0.250000    10.16667    0.05584    0.05584 =
         0.08627    0.00000    0.00000    0.02792
DFIX 0.8 0.05 N1 H1
DANG 1.1 0.1 H1 H1_$1
H1    3    0.933030    0.035346    0.172547    10.66667   -1.20000
C1    2    0.560124    0.000000    0.000000    10.50000    0.04764    0.07061 =
         0.05254   -0.02897   -0.01448    0.03531
AFIX  43
H2    3    0.429519   -0.000003    0.000002    10.50000   -1.20000
AFIX   0
HKLF 4

REM  nh4fe_c4_p02_s_test4 in P6(3)22
REM R1 =  0.0496 for     334 Fo > 4sig(Fo)  and  0.0682 for all     430 data
REM     22 parameters refined using      5 restraints

END

WGHT      0.0429      0.4770

REM Highest difference peak  0.673,  deepest hole -0.549,  1-sigma level  0.085
Q1    1   0.6667  0.3333  0.1233  10.33333  0.05    0.67
Q2    1   0.5931  0.1863  0.2500  10.50000  0.05    0.41
Q3    1   0.7135  0.2425  0.1659  11.00000  0.05    0.34
Q4    1   0.3333 -0.3333  0.2028  10.33333  0.05    0.33
Q5    1   0.6079  0.1919  0.1793  11.00000  0.05    0.32
Q6    1   0.7905  0.4952  0.2489  11.00000  0.05    0.29
Q7    1   1.0000  0.0000  0.0589  10.33333  0.05    0.26
Q8    1   0.8939  0.1061  0.2500  10.50000  0.05    0.26
Q9    1   0.6667  0.3333  0.0359  10.33333  0.05    0.25
Q10   1   1.0441  0.1371  0.2057  11.00000  0.05    0.25
Q11   1   0.3611  0.1373  0.0007  11.00000  0.05    0.24
Q12   1   0.3818 -0.2364  0.2500  10.50000  0.05    0.24
Q13   1   0.8107  0.1473  0.0667  11.00000  0.05    0.23
Q14   1   0.7734  0.2427  0.0955  11.00000  0.05    0.22
Q15   1   0.7113  0.1443  0.0543  11.00000  0.05    0.22
Q16   1   0.7852  0.0465  0.1745  11.00000  0.05    0.21
Q17   1   0.3454 -0.1129  0.2201  11.00000  0.05    0.21
Q18   1   0.3333 -0.3333  0.1245  10.33333  0.05    0.19
Q19   1   0.8608  0.2954  0.1049  11.00000  0.05    0.18
Q20   1   0.4729 -0.1912  0.2546  11.00000  0.05    0.17
;
_shelx_res_checksum              99234
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 0.6667 0.3333 0.2500 0.0353(4) Uani 1 6 d S T P
O1 O 0.6916(6) 0.1084(6) 0.1079(3) 0.0484(10) Uani 1 1 d . U .
N1 N 1.0000 0.0000 0.2500 0.066(3) Uani 1 6 d DS T P
H1 H 0.93(2) 0.04(3) 0.173(6) 0.079 Uiso 0.6667 1 d D U P
C1 C 0.5601(11) 0.0000 0.0000 0.054(2) Uani 1 2 d S TU P
H2 H 0.4295 0.0000 0.0000 0.065 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
Ni1 0.0434(6) 0.0434(6) 0.0190(5) 0.000 0.000 0.0217(3)
O1 0.060(3) 0.056(2) 0.0334(13) -0.0154(15) -0.0138(16) 0.032(2)
N1 0.056(5) 0.056(5) 0.086(9) 0.000 0.000 0.028(2)
C1 0.048(3) 0.071(5) 0.053(3) -0.029(4) -0.0145(19) 0.035(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.2312 0.4101 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0018 0.0018 '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'
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 82.32(19) . 10_665
O1 Ni1 O1 94.7(2) . 11_655
O1 Ni1 O1 91.82(13) 10_665 11_655
O1 Ni1 O1 91.82(13) . 2_655
O1 Ni1 O1 94.7(2) 10_665 2_655
O1 Ni1 O1 171.4(2) 11_655 2_655
O1 Ni1 O1 171.4(2) . 12
O1 Ni1 O1 91.82(13) 10_665 12
O1 Ni1 O1 91.82(13) 11_655 12
O1 Ni1 O1 82.32(19) 2_655 12
O1 Ni1 O1 91.82(13) . 3_665
O1 Ni1 O1 171.4(2) 10_665 3_665
O1 Ni1 O1 82.32(19) 11_655 3_665
O1 Ni1 O1 91.82(13) 2_655 3_665
O1 Ni1 O1 94.7(2) 12 3_665
C1 O1 Ni1 123.4(4) . .
O1 C1 O1 126.7(8) . 8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.047(4) .
Ni1 O1 2.047(4) 10_665
Ni1 O1 2.047(4) 11_655
Ni1 O1 2.047(4) 2_655
Ni1 O1 2.047(4) 12
Ni1 O1 2.047(4) 3_665
O1 C1 1.227(5) .
C1 O1 1.227(5) 8
