#------------------------------------------------------------------------------
#$Date: 2016-08-26 17:04:50 +0300 (Fri, 26 Aug 2016) $
#$Revision: 186029 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/91/7119178.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_7119178
loop_
_publ_author_name
'Jack Binns'
'Konstantin V. Kamenev'
'Katie E. R. Marriott'
'Garry J. McIntyre'
'Stephen A. Moggach'
'Mark Murrie'
'Simon Parsons'
_publ_section_title
;
 A non-topological mechanism for negative linear compressibility
;
_journal_name_full               Chem.Commun.
_journal_page_first              7486
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H8 Co3 K1 O14,O4'
_chemical_formula_sum            'C12 H8 Co3 K O18'
_chemical_formula_weight         656.08
_chemical_name_systematic        'potassium cobalt (II) citrate, UTSA-16'
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             14-07-21
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2016-05-13 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.0005(5)
_cell_length_b                   13.0005(5)
_cell_length_c                   30.2002(11)
_cell_measurement_reflns_used    4122
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     5104.2(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.784
_diffrn_measured_fraction_theta_max 0.739
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            7155
_diffrn_reflns_theta_full        18.080
_diffrn_reflns_theta_max         24.107
_diffrn_reflns_theta_min         3.720
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.164
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.14
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_details 'Flack (1983), 633 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9537
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1282
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.0015751
_refine_ls_shift/su_mean         0.0000722
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 18.6 29.7 17.5 6.83 1.60 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3531
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1485
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                1282
_reflns_number_total             1476
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0576
_oxford_refine_ls_scale          0.06335(4)
_oxford_reflns_number_all        1473
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'UTSA16 in I-42d'
_cod_data_source_file            c6cc02489k2.cif
_cod_data_source_block           SP3064_3kbar
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 4624 2016-04-14 12:54:50Z antanas 
;
_cod_original_sg_symbol_H-M      'I -4 2 d '
_cod_original_formula_sum        'C12 H8 Co3 K1 O18'
_cod_database_code               7119178
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT CO   (    1 ,X'S,U'S)  UNTIL O    (    7 ) 
CONT O    (    8 ,X'S,U[ISO]) 
CONT O    (    9 ,X'S,OCC)  UNTIL O    (   10 ) 
EQUIV O(9,OCC) O(10,OCC) 
WEIGHT -1 O(10,OCC) 
CONT ENANTIO 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(1) TO C(2) 
VIBR .0, 0.00200 = C(1) TO O(1) 
VIBR .0, 0.00200 = C(1) TO O(2) 
VIBR .0, 0.00500 = O(1) TO C(2) 
VIBR .0, 0.00500 = O(2) TO C(2) 
VIBR .0, 0.00500 = O(2) TO O(1) 
VIBR .0, 0.00200 = C(2) TO C(3) 
VIBR .0, 0.00500 = C(3) TO C(1) 
VIBR .0, 0.00200 = C(3) TO C(4) 
VIBR .0, 0.00200 = C(3) TO C(6) 
VIBR .0, 0.00200 = C(3) TO O(3) 
VIBR .0, 0.00500 = C(4) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(2) 
VIBR .0, 0.00500 = C(6) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(2) 
VIBR .0, 0.00500 = O(3) TO C(4) 
VIBR .0, 0.00500 = O(3) TO C(6) 
VIBR .0, 0.00200 = C(4) TO C(5) 
VIBR .0, 0.00500 = C(5) TO C(3) 
VIBR .0, 0.00200 = C(5) TO O(6) 
VIBR .0, 0.00200 = C(5) TO O(7) 
VIBR .0, 0.00500 = O(6) TO C(4) 
VIBR .0, 0.00500 = O(7) TO C(4) 
VIBR .0, 0.00500 = O(7) TO O(6) 
VIBR .0, 0.00200 = C(6) TO O(4) 
VIBR .0, 0.00200 = C(6) TO O(5) 
VIBR .0, 0.00500 = O(4) TO C(3) 
VIBR .0, 0.00500 = O(5) TO C(3) 
VIBR .0, 0.00500 = O(5) TO O(4) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(1) TO C(2) 
U(IJ) .0, 0.08000 = C(1) TO O(1) 
U(IJ) .0, 0.08000 = C(1) TO O(2) 
U(IJ) .0, 0.04000 = C(2) TO C(3) 
U(IJ) .0, 0.04000 = C(3) TO C(4) 
U(IJ) .0, 0.04000 = C(3) TO C(6) 
U(IJ) .0, 0.08000 = C(3) TO O(3) 
U(IJ) .0, 0.04000 = C(4) TO C(5) 
U(IJ) .0, 0.08000 = C(5) TO O(6) 
U(IJ) .0, 0.08000 = C(5) TO O(7) 
U(IJ) .0, 0.08000 = C(6) TO O(4) 
U(IJ) .0, 0.08000 = C(6) TO O(5) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
y,-x,-z
y+1/2,-x+1/2,-z+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
-y,x,-z
-y+1/2,x+1/2,-z+1/2
-x+1/2,y,-z+3/4
-x+1,y+1/2,-z+5/4
-y+1/2,-x,z+3/4
-y+1,-x+1/2,z+5/4
x+1/2,-y,-z+3/4
x+1,-y+1/2,-z+5/4
y+1/2,x,z+3/4
y+1,x+1/2,z+5/4
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Co1 Co 0.89540(11) 0.95131(11) 0.45964(3) 0.0203 1.0000 Uani . . . . . .
Co2 Co 1.0000 1.0000 0.30781(5) 0.0275 1.0000 Uani S T . . . .
K1 K 0.7500 0.8369(3) 0.3750 0.0436 1.0000 Uani S T . . . .
C1 C 1.1065(8) 0.9159(8) 0.3783(3) 0.0205 1.0000 Uani . U . . . .
C2 C 1.1502(9) 0.8328(9) 0.4082(3) 0.0284 1.0000 Uani . U . . . .
C3 C 1.0771(8) 0.8090(8) 0.4483(3) 0.0244 1.0000 Uani . U . . . .
C4 C 1.1400(9) 0.7335(9) 0.4767(3) 0.0269 1.0000 Uani . U . . . .
C5 C 1.0801(8) 0.6841(9) 0.5135(2) 0.0205 1.0000 Uani . U . . . .
C6 C 0.9785(9) 0.7557(9) 0.4314(3) 0.0280 1.0000 Uani . U . . . .
O1 O 1.1096(6) 1.0093(6) 0.39071(16) 0.0255 1.0000 Uani . U . . . .
O2 O 1.0697(6) 0.8893(6) 0.34092(18) 0.0303 1.0000 Uani . U . . . .
O3 O 1.0543(6) 0.9011(5) 0.47128(16) 0.0242 1.0000 Uani . U . . . .
O4 O 0.8952(6) 0.8011(6) 0.43768(19) 0.0240 1.0000 Uani . U . . . .
O5 O 0.9907(8) 0.6714(7) 0.4144(3) 0.0550 1.0000 Uani . U . . . .
O6 O 1.0373(6) 0.7368(6) 0.54193(18) 0.0327 1.0000 Uani . U . . . .
O7 O 1.0753(7) 0.5848(6) 0.5143(2) 0.0417 1.0000 Uani . U . . . .
O8 O 1.3097(19) 0.623(2) 0.5825(8) 0.176(9) 1.0000 Uiso . . . . . .
O9 O 1.178(2) 0.453(3) 0.4493(9) 0.1128 0.54(2) Uiso . . P . . .
O10 O 1.097(3) 0.490(3) 0.4298(10) 0.1180 0.46(2) Uiso . . P . . .
H21 H 1.2171 0.8561 0.4192 0.0284 1.0000 Uiso R . . . . .
H22 H 1.1581 0.7701 0.3916 0.0278 1.0000 Uiso R . . . . .
H41 H 1.1946 0.7726 0.4899 0.0280 1.0000 Uiso R . . . . .
H42 H 1.1697 0.6810 0.4586 0.0281 1.0000 Uiso R . . . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 5_775 Co1 . O3 3_576 168.2(3) yes
O1 5_775 Co1 . O6 3_576 86.0(3) yes
O3 3_576 Co1 . O6 3_576 93.5(2) yes
O1 5_775 Co1 . O3 5_775 87.3(2) yes
O3 3_576 Co1 . O3 5_775 81.4(2) yes
O6 3_576 Co1 . O3 5_775 104.7(3) yes
O1 5_775 Co1 . Co1 5_775 85.8(2) yes
O3 3_576 Co1 . Co1 5_775 89.0(2) yes
O6 3_576 Co1 . Co1 5_775 150.9(2) yes
O3 5_775 Co1 . Co1 5_775 47.0(2) yes
O1 5_775 Co1 . Co1 3_576 126.3(2) yes
O3 3_576 Co1 . Co1 3_576 42.3(2) yes
O6 3_576 Co1 . Co1 3_576 101.4(2) yes
O3 5_775 Co1 . Co1 3_576 39.15(14) yes
Co1 5_775 Co1 . Co1 3_576 62.34(2) yes
O1 5_775 Co1 . Co1 7_756 143.6(2) yes
O3 3_576 Co1 . Co1 7_756 38.45(19) yes
O6 3_576 Co1 . Co1 7_756 130.42(17) yes
O3 5_775 Co1 . Co1 7_756 83.39(17) yes
Co1 5_775 Co1 . Co1 7_756 62.34(2) yes
O1 5_775 Co1 . O3 . 104.8(2) yes
O3 3_576 Co1 . O3 . 78.2(2) yes
O6 3_576 Co1 . O3 . 164.5(3) yes
O3 5_775 Co1 . O3 . 87.2(3) yes
Co1 5_775 Co1 . O3 . 43.31(18) yes
O1 5_775 Co1 . O4 . 85.1(3) yes
O3 3_576 Co1 . O4 . 106.7(3) yes
O6 3_576 Co1 . O4 . 93.4(3) yes
O3 5_775 Co1 . O4 . 159.8(3) yes
Co1 5_775 Co1 . O4 . 113.6(2) yes
Co1 3_576 Co1 . Co1 7_756 55.31(4) yes
Co1 3_576 Co1 . O3 . 81.43(16) yes
Co1 7_756 Co1 . O3 . 39.81(13) yes
Co1 3_576 Co1 . O4 . 145.78(18) yes
Co1 7_756 Co1 . O4 . 91.7(2) yes
O3 . Co1 . O4 . 76.8(3) yes
O7 15_554 Co2 . O7 11_674 96.6(5) yes
O7 15_554 Co2 . O2 5_775 103.4(3) yes
O7 11_674 Co2 . O2 5_775 116.3(3) yes
O7 15_554 Co2 . O2 . 116.3(3) yes
O7 11_674 Co2 . O2 . 103.4(3) yes
O2 5_775 Co2 . O2 . 119.1(4) yes
C2 . C1 . O1 . 119.6(8) yes
C2 . C1 . O2 . 118.3(9) yes
O1 . C1 . O2 . 122.1(9) yes
C1 . C2 . C3 . 111.8(9) yes
C1 . C2 . H21 . 108.2 no
C3 . C2 . H21 . 109.7 no
C1 . C2 . H22 . 109.6 no
C3 . C2 . H22 . 107.4 no
H21 . C2 . H22 . 110.1 no
C2 . C3 . C4 . 103.5(8) yes
C2 . C3 . C6 . 109.6(7) yes
C4 . C3 . C6 . 109.8(9) yes
C2 . C3 . O3 . 109.8(8) yes
C4 . C3 . O3 . 112.2(7) yes
C6 . C3 . O3 . 111.6(9) yes
C3 . C4 . C5 . 114.1(9) yes
C3 . C4 . H41 . 106.6 no
C5 . C4 . H41 . 107.7 no
C3 . C4 . H42 . 110.6 no
C5 . C4 . H42 . 109.1 no
H41 . C4 . H42 . 108.5 no
C4 . C5 . O6 . 120.9(11) yes
C4 . C5 . O7 . 117.8(9) yes
O6 . C5 . O7 . 121.3(8) yes
C3 . C6 . O4 . 117.3(9) yes
C3 . C6 . O5 . 115.7(10) yes
O4 . C6 . O5 . 127.0(11) yes
Co1 5_775 O1 . C1 . 120.8(5) yes
Co2 . O2 . C1 . 115.1(7) yes
Co1 . O3 . Co1 7_756 97.9(3) yes
Co1 . O3 . C3 . 111.7(6) yes
Co1 7_756 O3 . C3 . 117.8(5) yes
Co1 . O3 . Co1 5_775 89.7(3) yes
Co1 7_756 O3 . Co1 5_775 102.4(3) yes
C3 . O3 . Co1 5_775 129.7(5) yes
Co1 . O4 . C6 . 119.7(7) yes
Co1 7_756 O6 . C5 . 120.4(7) yes
Co2 12_664 O7 . C5 . 126.4(6) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 . O1 5_775 2.145(5) yes
Co1 . O3 3_576 2.089(5) yes
Co1 . O6 3_576 2.068(8) yes
Co1 . O3 5_775 2.058(7) yes
Co1 . Co1 5_775 3.000(3) yes
Co1 . Co1 3_576 3.2316(19) yes
Co1 . Co1 7_756 3.2316(19) yes
Co1 . O3 . 2.195(7) yes
Co1 . O4 . 2.062(7) yes
Co2 . O7 15_554 1.976(7) yes
Co2 . O7 11_674 1.976(7) yes
Co2 . O2 5_775 1.972(7) yes
Co2 . O2 . 1.972(7) yes
C1 . C2 . 1.517(14) yes
C1 . O1 . 1.272(13) yes
C1 . O2 . 1.274(11) yes
C2 . C3 . 1.571(13) yes
C2 . H21 . 0.980 no
C2 . H22 . 0.961 no
C3 . C4 . 1.540(14) yes
C3 . C6 . 1.544(15) yes
C3 . O3 . 1.415(12) yes
C4 . C5 . 1.500(14) yes
C4 . H41 . 0.959 no
C4 . H42 . 0.955 no
C5 . O6 . 1.232(12) yes
C5 . O7 . 1.293(15) yes
C6 . O4 . 1.248(13) yes
C6 . O5 . 1.221(14) yes
