#------------------------------------------------------------------------------
#$Date: 2017-01-09 05:02:49 +0200 (Mon, 09 Jan 2017) $
#$Revision: 190064 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/68/7226835.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_7226835
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                   7.26097(16)
_cell_length_b                   7.26097(16)
_cell_length_c                   8.0811(2)
_cell_measurement_reflns_used    4923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7310
_cell_measurement_theta_min      3.2000
_cell_volume                     368.969(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.9961
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measurement_device_type  MAR345dbt
_diffrn_measurement_method       'Phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7561
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.785
_diffrn_reflns_theta_min         3.240
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    2.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.75759
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 104 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         361
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0271P)²+0.1336P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0477
_reflns_Friedel_coverage         0.438
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                351
_reflns_number_total             361
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01891b2.cif
_cod_data_source_block           ANiF_100K
_cod_depositor_comments
'Adding full bibliography for 7226831--7226836.cif.'
_cod_original_cell_volume        368.969(19)
_cod_database_code               7226835
_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 NH4Ni_120sec_test1 in P6(3)22
REM P6(3)22 (#182 in standard setting)
CELL 0.71073   7.260970   7.260970   8.081097  90.0000  90.0000 120.0000
ZERR    2.00   0.000157   0.000157   0.000206   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
UNIT 2.000 6 14 12 2.000
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
ACTA
L.S. 4
BOND
FMAP 2
PLAN 20

EQIV $1 -y, -x, 1/2-z

WGHT    0.027100    0.133600
FVAR       1.01274
MOLE   1
NI1   1    0.666667    0.333333    0.250000    10.16667    0.00608    0.00608 =
         0.00535    0.00000    0.00000    0.00304
O1    4    0.691523    0.111408    0.106679    11.00000    0.01285    0.01033 =
         0.00999   -0.00499   -0.00341    0.00687
N1    5    0.000000    0.000000    0.207699    10.16667    0.01080    0.01080 =
         0.01735    0.00000    0.00000    0.00540
H1    3   -0.110011    0.032865    0.163015    10.50000    0.04724
DFIX 0.9 0.2 N1 H2_$1
H2    3    0.000000    0.000000    0.158721    10.16667   -1.20000
C1    2    0.556385    0.000000    0.000000    10.50000    0.01013    0.01099 =
         0.01926   -0.00643   -0.00321    0.00550
AFIX  43
H3    3    0.428303    0.000000    0.000000    10.50000   -1.50000
REM #####
AFIX   0
HKLF 4

REM  NH4Ni_120sec_test1 in P6(3)22
REM R1 =  0.0179 for     351 Fo > 4sig(Fo)  and  0.0188 for all     361 data
REM     25 parameters refined using      0 restraints

END

WGHT      0.0271      0.1329

REM Highest difference peak  0.251,  deepest hole -0.457,  1-sigma level  0.058
Q1    1   0.7209  0.2446  0.1401  11.00000  0.05    0.25
Q2    1   0.6268  0.1835  0.1508  11.00000  0.05    0.23
Q3    1   0.6667  0.3333  0.1012  10.33333  0.05    0.17
Q4    1   0.8152  0.1924 -0.0195  11.00000  0.05    0.16
Q5    1   0.7822  0.1030  0.0554  11.00000  0.05    0.15
Q6    1   0.6667  0.3333 -0.0047  10.33333  0.05    0.15
Q7    1   0.5264  0.0422  0.1551  11.00000  0.05    0.14
Q8    1   0.7603  0.5205  0.2500  10.50000  0.05    0.13
Q9    1  -0.2439 -0.0187  0.0369  11.00000  0.05    0.13
Q10   1   0.3451 -0.0438  0.0935  11.00000  0.05    0.13
Q11   1   0.7681  0.0557  0.1472  11.00000  0.05    0.13
Q12   1   0.3333 -0.3333  0.0946  10.33333  0.05    0.12
Q13   1   0.5982 -0.0563  0.1292  11.00000  0.05    0.12
Q14   1   0.6803  0.0565  0.2340  11.00000  0.05    0.12
Q15   1  -0.1421 -0.0457  0.1938  11.00000  0.05    0.12
Q16   1   0.4844 -0.2578  0.2500  10.50000  0.05    0.11
Q17   1   0.5997  0.0746  0.2294  11.00000  0.05    0.11
Q18   1   0.5071 -0.1851  0.1444  11.00000  0.05    0.11
Q19   1  -0.2215 -0.1306  0.0282  11.00000  0.05    0.10
Q20   1   0.4535 -0.0931  0.2500  10.50000  0.05    0.10
;
_shelx_res_checksum              28367
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 0.00583(17) Uani 1 6 d S T P
O1 O 0.6915(2) 0.1114(2) 0.10668(14) 0.0106(3) Uani 1 1 d . . .
N1 N 0.0000 0.0000 0.2077(6) 0.0130(11) Uani 0.5 3 d DS T P
H1 H -0.110(10) 0.033(11) 0.163(7) 0.047(19) Uiso 0.5 1 d . . P
H2 H 0.0000 0.0000 0.159(16) 0.057 Uiso 0.5 3 d S U P
C1 C 0.5564(4) 0.0000 0.0000 0.0134(5) Uani 1 2 d S T P
H3 H 0.4283 0.0000 0.0000 0.020 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 0.00608(19) 0.00608(19) 0.0053(2) 0.000 0.000 0.00304(9)
O1 0.0129(6) 0.0103(6) 0.0100(5) -0.0050(5) -0.0034(5) 0.0069(6)
N1 0.0108(11) 0.0108(11) 0.017(3) 0.000 0.000 0.0054(6)
C1 0.0101(8) 0.0110(11) 0.0193(11) -0.0064(11) -0.0032(6) 0.0055(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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 82.52(7) . 10_665
O1 Ni1 O1 94.93(7) . 11_655
O1 Ni1 O1 91.59(5) 10_665 11_655
O1 Ni1 O1 91.59(5) . 2_655
O1 Ni1 O1 94.93(7) 10_665 2_655
O1 Ni1 O1 171.32(7) 11_655 2_655
O1 Ni1 O1 171.32(7) . 12
O1 Ni1 O1 91.59(5) 10_665 12
O1 Ni1 O1 91.59(5) 11_655 12
O1 Ni1 O1 82.52(7) 2_655 12
O1 Ni1 O1 91.59(5) . 3_665
O1 Ni1 O1 171.32(7) 10_665 3_665
O1 Ni1 O1 82.52(7) 11_655 3_665
O1 Ni1 O1 91.59(5) 2_655 3_665
O1 Ni1 O1 94.93(7) 12 3_665
C1 O1 Ni1 123.00(14) . .
O1 C1 O1 125.1(3) 8 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.0643(12) .
Ni1 O1 2.0643(12) 10_665
Ni1 O1 2.0643(12) 11_655
Ni1 O1 2.0643(12) 2_655
Ni1 O1 2.0643(12) 12
Ni1 O1 2.0643(12) 3_665
O1 C1 1.2516(17) .
N1 N1 0.684(10) 10
C1 O1 1.2516(17) 8
