#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:42:55 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179859 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/55/7015501.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_7015501
loop_
_publ_author_name
'Saines, Paul J.'
'Yeung, Hamish H.-M.'
'Hester, James R.'
'Lennie, Alistair R.'
'Cheetham, Anthony K.'
_publ_section_title
;
 Detailed investigations of phase transitions and magnetic structure in
 Fe(iii), Mn(ii), Co(ii) and Ni(ii) 3,4,5-trihydroxybenzoate (gallate)
 dihydrates by neutron and X-ray diffraction.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6401
_journal_page_last               6410
_journal_paper_doi               10.1039/c0dt01687j
_journal_volume                  40
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C7 H4 Ni O5, 2(H2 O)'
_chemical_formula_sum            'C7 H8 Ni O7'
_chemical_formula_weight         262.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-11-10T10:01:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.8079(3)
_cell_length_b                   8.8079(3)
_cell_length_c                   21.1663(6)
_cell_measurement_reflns_used    6087
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.1629
_cell_measurement_theta_min      2.8319
_cell_measurement_wavelength     0.71073
_cell_volume                     1422.07(8)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction, 2010'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction, 2010'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction, 2010'
_computing_molecular_graphics    'Diamond (Brandenburg 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16110
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         2.84
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.065
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.0831
_exptl_crystal_size_min          0.0561
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2410
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0310P)²+1.2462P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                2204
_reflns_number_total             2410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01687j.txt
_cod_data_source_block           nigallate_p1
_cod_original_cell_volume        1422.06(7)
_cod_database_code               7015501
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
'y, x, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.03473(3) 0.98102(3) 0.082815(12) 0.00732(8) Uani 1 1 d . . .
O6 O 0.0986(2) 1.0986(2) 0 0.0116(4) Uani 1 2 d S . .
O8 O -0.2142(2) 0.8113(2) 0.05265(7) 0.0111(3) Uani 1 1 d . . .
O1 O 0 0.8714(2) 0.1667 0.0104(4) Uani 1 2 d S . .
O7 O 0.3035(2) 1.1736(2) 0.09919(7) 0.0149(4) Uani 1 1 d D . .
O3 O -0.0393(2) 1.1520(2) 0.11524(7) 0.0121(3) Uani 1 1 d . . .
O2 O 0.1021(2) 0.7829(2) 0.06322(7) 0.0140(3) Uani 1 1 d D . .
C1 C 0 0.7205(4) 0.1667 0.0099(7) Uani 1 2 d S . .
C3 C 0 1.2366(4) 0.1667 0.0117(7) Uani 1 2 d S . .
C8 C -0.2670(4) 0.7330(4) 0 0.0118(7) Uani 1 2 d S . .
C6 C 0.2492(4) 1.2492(4) 0 0.0104(6) Uani 1 2 d S . .
C9 C -0.4354(4) 0.5646(4) 0 0.0124(6) Uani 1 2 d S . .
C7 C 0.3624(3) 1.2977(3) 0.05180(10) 0.0121(5) Uani 1 1 d D . .
O9 O 0.6816(3) 0.1339(3) 0.04806(8) 0.0261(4) Uani 1 1 d D . .
O10 O 0.5288(2) 0.8070(3) 0.12579(8) 0.0264(4) Uani 1 1 d D . .
C5 C 0.0477(3) 1.5071(3) 0.11181(11) 0.0130(5) Uani 1 1 d . . .
H5 H 0.0779 1.4679 0.0746 0.016 Uiso 1 1 calc R . .
C10 C -0.4817(3) 0.4553(3) 0.05286(11) 0.0131(5) Uani 1 1 d . . .
H10 H -0.4074 0.4888 0.0888 0.016 Uiso 1 1 calc R . .
C2 C 0.0504(3) 0.6661(3) 0.11235(10) 0.0119(5) Uani 1 1 d D . .
C4 C 0 1.4056(4) 0.1667 0.0136(7) Uani 1 2 d S . .
H10A H 0.424(2) 0.718(4) 0.1187(18) 0.094(8) Uiso 1 1 d D . .
H10B H 0.602(4) 0.801(5) 0.0992(16) 0.094(8) Uiso 1 1 d D . .
H9B H 0.776(3) 0.158(5) 0.0693(17) 0.094(8) Uiso 1 1 d D . .
H9A H 0.590(3) 0.045(4) 0.0658(17) 0.094(8) Uiso 1 1 d D . .
H7 H 0.364(3) 1.214(3) 0.1331(7) 0.032(8) Uiso 1 1 d D . .
H2 H 0.116(4) 0.746(3) 0.0276(6) 0.034(9) Uiso 1 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
_geom_angle_publ_flag
O6 Ni1 O1 173.28(5) . . ?
O6 Ni1 O3 91.37(5) . . ?
O1 Ni1 O3 91.74(7) . . ?
O6 Ni1 O8 91.51(7) . . ?
O1 Ni1 O8 94.37(4) . . ?
O3 Ni1 O8 91.33(7) . . ?
O6 Ni1 O7 79.37(7) . . ?
O1 Ni1 O7 94.68(4) . . ?
O3 Ni1 O7 89.74(6) . . ?
O8 Ni1 O7 170.85(6) . . ?
O6 Ni1 O2 97.65(4) . . ?
O1 Ni1 O2 79.26(7) . . ?
O3 Ni1 O2 170.97(6) . . ?
O8 Ni1 O2 88.67(6) . . ?
O7 Ni1 O2 91.70(7) . . ?
C6 O6 Ni1 113.94(6) . . ?
C6 O6 Ni1 113.94(6) . 6_465 ?
Ni1 O6 Ni1 132.13(11) . 6_465 ?
C8 O8 Ni1 129.74(16) . . ?
C1 O1 Ni1 114.37(5) . 5 ?
C1 O1 Ni1 114.37(5) . . ?
Ni1 O1 Ni1 131.25(11) 5 . ?
C7 O7 Ni1 109.80(13) . . ?
C3 O3 Ni1 129.12(16) . . ?
C2 O2 Ni1 109.89(13) . . ?
O1 C1 C2 120.05(15) . 5 ?
O1 C1 C2 120.05(15) . . ?
C2 C1 C2 119.9(3) 5 . ?
O3 C3 O3 126.3(3) 5 . ?
O3 C3 C4 116.86(15) 5 . ?
O3 C3 C4 116.86(15) . . ?
O8 C8 O8 125.9(3) 6_465 . ?
O8 C8 C9 117.05(15) 6_465 . ?
O8 C8 C9 117.05(15) . . ?
O6 C6 C7 120.64(15) . . ?
O6 C6 C7 120.64(15) . 6_465 ?
C7 C6 C7 118.7(3) . 6_465 ?
C10 C9 C10 121.2(3) 6_465 . ?
C10 C9 C8 119.38(16) 6_465 . ?
C10 C9 C8 119.38(16) . . ?
O7 C7 C10 125.2(2) . 1_665 ?
O7 C7 C6 113.6(2) . . ?
C10 C7 C6 121.3(2) 1_665 . ?
C2 C5 C4 119.2(2) 1_565 . ?
C7 C10 C9 118.7(2) 1_445 . ?
O2 C2 C5 125.6(2) . 1_545 ?
O2 C2 C1 114.2(2) . . ?
C5 C2 C1 120.2(2) 1_545 . ?
C5 C4 C5 121.3(3) . 5 ?
C5 C4 C3 119.36(15) . . ?
C5 C4 C3 119.36(15) 5 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O6 1.9695(9) . ?
Ni1 O1 1.9701(9) . ?
Ni1 O3 2.0359(15) . ?
Ni1 O8 2.0424(16) . ?
Ni1 O7 2.1412(16) . ?
Ni1 O2 2.1463(16) . ?
O6 C6 1.326(4) . ?
O6 Ni1 1.9696(9) 6_465 ?
O8 C8 1.270(2) . ?
O1 C1 1.328(4) . ?
O1 Ni1 1.9701(9) 5 ?
O7 C7 1.380(3) . ?
O3 C3 1.266(2) . ?
O2 C2 1.370(3) . ?
C1 C2 1.401(3) 5 ?
C1 C2 1.401(3) . ?
C3 O3 1.266(2) 5 ?
C3 C4 1.489(5) . ?
C8 O8 1.270(2) 6_465 ?
C8 C9 1.483(5) . ?
C6 C7 1.397(3) . ?
C6 C7 1.397(3) 6_465 ?
C9 C10 1.397(3) 6_465 ?
C9 C10 1.397(3) . ?
C7 C10 1.381(3) 1_665 ?
C5 C2 1.389(3) 1_565 ?
C5 C4 1.396(3) . ?
C10 C7 1.381(3) 1_445 ?
C2 C5 1.389(3) 1_545 ?
C4 C5 1.396(3) 5 ?
