#------------------------------------------------------------------------------
#$Date: 2017-01-09 04:02:49 +0100 (lun 09 de ene de 2017) $
#$Revision: 190064 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/68/7226831.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_7226831
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'
_chemical_properties_physical    ', Moisture-sensitive'
_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                   7.1610(2)
_cell_length_b                   7.1610(2)
_cell_length_c                   8.0474(4)
_cell_measurement_reflns_used    487
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.9280
_cell_measurement_theta_min      1.9010
_cell_volume                     357.38(2)
_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 0.93 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.743
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.743
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1185
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.695
_diffrn_reflns_theta_full        14.301
_diffrn_reflns_theta_max         20.792
_diffrn_reflns_theta_min         1.902
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58169
_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    1.968
_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         0.805
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.234
_refine_ls_abs_structure_details
;
 Flack x determined using 103 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         459
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0499
_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)+(0.0536P)²+0.2952P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.417
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.603
_reflns_number_gt                382
_reflns_number_total             459
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01891b2.cif
_cod_data_source_block           ANiF_p01
_cod_depositor_comments
'Adding full bibliography for 7226831--7226836.cif.'
_cod_original_cell_volume        357.38(3)
_cod_database_code               7226831
_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_p01_s_test15 in P6(3)22
REM P6(3)22 (#182 in standard setting)
CELL 0.41168   7.160998   7.160998   8.047413  90.0000  90.0000 120.0000
ZERR    2.00   0.000228   0.000228   0.000351   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

ACTA
LIST 4

L.S. 20
BOND
FMAP 2
PLAN 20

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

WGHT    0.053600    0.295200
FVAR      11.42103
NI1   1    0.666667    0.333333    0.250000    10.16667    0.03309    0.03309 =
         0.01643    0.00000    0.00000    0.01655
O1    4    0.691270    0.109165    0.106960    11.00000    0.04751    0.04411 =
         0.03318   -0.01314   -0.01312    0.02456
N1    5    1.000000    0.000000    0.250000    10.16667    0.04070    0.04070 =
         0.10142    0.00000    0.00000    0.02035
DFIX 0.8 0.01 N1 H1
DANG 1.1 0.04 H1 H1_$1
H1    3    0.937058    0.041232    0.191886    10.66667   -1.20000
C1    2    0.559858    0.000000    0.000000    10.50000    0.04105    0.05910 =
         0.04586   -0.02590   -0.01295    0.02955
AFIX  43
H2    3    0.429987   -0.000001   -0.000001    10.50000   -1.20000
REM #####
REM #####
REM #####
REM #####

REM #####

REM #####
AFIX   0
HKLF 4

REM  nh4fe_c4_p01_s_test15 in P6(3)22
REM R1 =  0.0499 for     382 Fo > 4sig(Fo)  and  0.0604 for all     459 data
REM     22 parameters refined using      5 restraints

END

WGHT      0.0536      0.2953

REM Highest difference peak  0.805,  deepest hole -0.870,  1-sigma level  0.234
Q1    1   0.3754 -0.2491  0.2500  10.50000  0.05    0.81
Q2    1   0.3333 -0.3333  0.1994  10.33333  0.05    0.73
Q3    1   0.5089  0.1984  0.2523  11.00000  0.05    0.66
Q4    1   0.9205  0.0795  0.2500  10.50000  0.05    0.61
Q5    1   0.8975 -0.0587  0.1943  11.00000  0.05    0.61
Q6    1   0.6149  0.2146  0.1788  11.00000  0.05    0.59
Q7    1   0.7285  0.4580  0.1706  11.00000  0.05    0.58
Q8    1   0.8441 -0.0779  0.2500  10.50000  0.05    0.55
Q9    1   0.7062  0.0000  0.0000  10.50000  0.05    0.54
Q10   1   0.8408  0.2097 -0.0175  11.00000  0.05    0.49
Q11   1   0.3734  0.0569  0.0182  11.00000  0.05    0.44
Q12   1   0.3388 -0.0277  0.0636  11.00000  0.05    0.43
Q13   1   0.6127 -0.0195  0.0624  11.00000  0.05    0.40
Q14   1   0.3045  0.0000  0.0000  10.50000  0.05    0.39
Q15   1   0.7726  0.1070  0.0332  11.00000  0.05    0.37
Q16   1   0.4134 -0.1601  0.1881  11.00000  0.05    0.32
Q17   1   0.7158 -0.1462  0.0832  11.00000  0.05    0.30
Q18   1   0.4342  0.0969  0.0994  11.00000  0.05    0.30
Q19   1   0.5452 -0.1437  0.1032  11.00000  0.05    0.26
Q20   1   0.5385  0.0694  0.0703  11.00000  0.05    0.25
;
_shelx_res_checksum              16352
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 0.0275(4) Uani 1 6 d S T P
O1 O 0.6913(5) 0.1092(5) 0.1070(5) 0.0409(8) Uani 1 1 d . U .
N1 N 1.0000 0.0000 0.2500 0.061(3) Uani 1 6 d DS T P
H1 H 0.94(2) 0.04(2) 0.192(5) 0.073 Uiso 0.6667 1 d D U P
C1 C 0.5599(9) 0.0000 0.0000 0.0467(18) Uani 1 2 d S TU P
H2 H 0.4300 0.0000 0.0000 0.056 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 0.0331(5) 0.0331(5) 0.0164(6) 0.000 0.000 0.0165(2)
O1 0.0475(19) 0.0441(17) 0.033(2) -0.0131(13) -0.0131(14) 0.0246(16)
N1 0.041(3) 0.041(3) 0.101(11) 0.000 0.000 0.0204(15)
C1 0.041(2) 0.059(4) 0.046(5) -0.026(3) -0.0130(17) 0.0295(19)
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 82.58(18) . 10_665
O1 Ni1 O1 94.8(2) . 11_655
O1 Ni1 O1 91.64(14) 10_665 11_655
O1 Ni1 O1 91.64(14) . 2_655
O1 Ni1 O1 94.8(2) 10_665 2_655
O1 Ni1 O1 171.48(18) 11_655 2_655
O1 Ni1 O1 171.48(18) . 12
O1 Ni1 O1 91.64(14) 10_665 12
O1 Ni1 O1 91.64(15) 11_655 12
O1 Ni1 O1 82.58(18) 2_655 12
O1 Ni1 O1 91.64(15) . 3_665
O1 Ni1 O1 171.48(18) 10_665 3_665
O1 Ni1 O1 82.58(18) 11_655 3_665
O1 Ni1 O1 91.64(14) 2_655 3_665
O1 Ni1 O1 94.8(2) 12 3_665
C1 O1 Ni1 123.6(4) . .
O1 C1 O1 126.6(7) 8 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.053(3) .
Ni1 O1 2.053(3) 10_665
Ni1 O1 2.053(3) 11_655
Ni1 O1 2.053(3) 2_655
Ni1 O1 2.053(3) 12
Ni1 O1 2.053(3) 3_665
O1 C1 1.226(4) .
C1 O1 1.225(4) 8
