#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010397.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2010397
loop_
_publ_author_name
'Henderson, W.'
'Nicholson, B.K.'
_publ_section_title
;
 Hexaaquanickel(II) <small>D</small>-Camphor-10-sulfonate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              37
_journal_page_last               40
_journal_paper_doi               10.1107/S0108270194006542
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C20 H42 Ni1 O14 S2'
_chemical_formula_sum            'C20 H42 Ni O14 S2'
_chemical_formula_weight         629.37
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_type_scat_source           'SHELXL93 (Sheldrick, 1993)'
_cell_angle_alpha                90.
_cell_angle_beta                 94.22(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            2
_cell_length_a                   11.677(2)
_cell_length_b                   7.064(2)
_cell_length_c                   17.078(2)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    143
_cell_measurement_theta_max      28
_cell_measurement_theta_min      10
_cell_volume                     1404.9(5)
_diffrn_measurement_device       'Nicolet R3'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2834
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0.993-1.006
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.90
_exptl_absorpt_correction_T_max  0.674
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale blue-green'
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       tablet
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.038
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     375
_refine_ls_number_reflns         2694
_refine_ls_R_factor_obs          0.0491
_refine_ls_shift/esd_max         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; w = [\s^2^(F~o~^2^) + (0.0440P)^2^ + 0.15P]
where P = [max(F~o~^2^,0) + 2F~c~^2^]/3
;
_refine_ls_wR_factor_obs         0.0721
_reflns_number_observed          2222
_reflns_number_total             2694
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            oh1067.cif
_cod_data_source_block           oh1067_structure_1_of_1
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C20 H42 Ni1 O14 S2'
_cod_database_code               2010397
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Ni(1) .75870(10) .0000 .00590(10) .012(1)
O(1) .6674(4) .2152(7) .0523(3) .016(1)
O(2) .6504(2) -.0004(9) -.0926(2) .018(1)
O(3) .8517(4) -.2151(7) -.0422(3) .016(1)
O(4) .8647(2) -.0025(8) .1064(2) .018(1)
O(5) .6669(4) -.2197(7) .0494(3) .016(1)
O(6) .8496(4) .2213(7) -.0374(3) .016(1)
S(1) .08220(10) .0022(3) .83550(10) .012(1)
O(11) .2013(2) .0001(8) .8695(2) .016(1)
O(12) .0188(4) .1686(6) .8600(3) .016(1)
O(13) .0212(4) -.1745(6) .8488(3) .015(1)
O(14) .1232(3) .0704(6) .5729(2) .029(1)
C(11) -.0063(3) -.0138(11) .6744(2) .013(1)
C(12) .0268(4) .0431(7) .5926(3) .020(1)
C(13) -.0845(4) .0554(8) .5396(3) .023(1)
C(14) -.1734(3) .0000(12) .5968(2) .017(1)
C(15) -.1578(4) -.2155(8) .6122(3) .020(1)
C(16) -.0415(4) -.2242(8) .6627(3) .016(1)
C(17) -.1259(4) .0878(8) .6764(3) .015(1)
C(18) -.1996(4) .0326(9) .7434(2) .019(1)
C(19) -.1154(5) .3045(8) .6734(3) .024(1)
C(110) .0955(4) .0270(10) .7331(2) .014(1)
S(2) .40800(10) -.0002(3) .14770(10) .012(1)
O(21) .2853(2) .0007(9) .1221(2) .016(1)
O(22) .4665(4) -.1723(6) .1247(3) .017(1)
O(23) .4678(4) .1702(6) .1241(3) .015(1)
O(24) .4618(4) -.2454(7) .3836(2) .024(1)
C(21) .5300(3) .0043(12) .2984(2) .015(1)
C(22) .5293(5) -.1224(8) .3721(3) .019(1)
C(23) .6301(5) -.0570(8) .4274(3) .023(1)
C(24) .6815(4) .1042(8) .3803(3) .017(1)
C(25) .7412(3) .0085(13) .3130(2) .021(1)
C(26) .6388(4) -.0655(7) .2583(3) .015(1)
C(27) .5714(4) .1936(8) .3370(3) .016(1)
C(28) .5994(4) .3517(8) .2798(3) .019(1)
C(29) .4910(5) .2765(10) .3941(4) .024(2)
C(210) .4126(3) -.0007(12) .2519(2) .015(1)
H(11) .708(5) .296(7) .081(3) .025(4)
H(12) .600(3) .209(10) .070(3) .025(4)
H(21) .609(5) -.097(7) -.111(3) .025(4)
H(22) .595(4) .083(7) -.096(3) .025(4)
H(31) .810(5) -.299(8) -.067(4) .025(4)
H(32) .898(4) -.178(9) -.077(3) .025(4)
H(41) .917(4) .083(7) .106(3) .025(4)
H(42) .899(5) -.104(6) .124(3) .025(4)
H(51) .700(5) -.312(7) .076(3) .025(4)
H(52) .616(4) -.178(9) .078(3) .025(4)
H(61) .802(4) .304(8) -.057(4) .025(4)
H(62) .903(4) .223(10) -.069(3) .025(4)
H(13A) -.0978(4) .1851(8) .5190(3) .028
H(13B) -.0842(4) -.0346(8) .4951(3) .028
H(14) -.2538(3) .0385(12) .5798(2) .021
H(15A) -.1538(4) -.2863(8) .5625(3) .024
H(15B) -.2211(4) -.2670(8) .6413(3) .024
H(16A) -.0510(4) -.2864(8) .7138(3) .019
H(16B) .0167(4) -.2945(8) .6350(3) .019
H(18A) -.177(2) .109(4) .7899(7) .029
H(18B) -.188(2) -.1019(15) .7557(13) .029
H(18C) -.2807(5) .056(5) .7273(8) .029
H(19A) -.066(2) .3401(8) .6320(14) .036
H(19B) -.082(3) .3514(9) .7241(7) .036
H(19C) -.1917(6) .3602(8) .662(2) .036
H(11A) .1201(4) .1587(10) .7239(2) .017
H(11B) .1592(4) -.0564(10) .7194(2) .017
H(23A) .6864(5) -.1603(8) .4382(3) .028
H(23B) .6038(5) -.0101(8) .4776(3) .028
H(24) .7307(4) .1953(8) .4125(3) .021
H(25A) .7911(3) -.0969(13) .3329(3) .026
H(25B) .7878(3) .1006(13) .2854(2) .026
H(26A) .6401(4) -.2054(7) .2549(3) .018
H(26B) .6407(4) -.0120(7) .2049(3) .018
H(28A) .648(2) .3009(13) .2401(11) .029
H(28B) .641(2) .454(2) .3088(4) .029
H(28C) .5279(4) .402(3) .2540(14) .029
H(29A) .5329(9) .368(4) .4284(14) .035
H(29B) .461(2) .1746(12) .4260(15) .035
H(29C) .4268(17) .340(5) .3647(4) .035
H(21A) .3681(3) .1099(12) .2683(2) .018
H(21B) .3718(3) -.1154(12) .2682(2) .018
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(2) Ni(1) O(4) 178.7(2) yes
O(4) Ni(1) O(1) 88.9(2) yes
O(4) Ni(1) O(5) 89.4(2) yes
O(2) Ni(1) O(6) 90.5(2) yes
O(1) Ni(1) O(6) 82.7(2) yes
O(2) Ni(1) O(3) 89.0(2) yes
O(1) Ni(1) O(3) 179.2(2) yes
O(6) Ni(1) O(3) 96.6(2) yes
O(2) Ni(1) O(1) 90.7(2) yes
O(2) Ni(1) O(5) 89.4(2) yes
O(1) Ni(1) O(5) 96.9(2) yes
O(4) Ni(1) O(6) 90.7(2) yes
O(5) Ni(1) O(6) 179.6(2) yes
O(4) Ni(1) O(3) 91.4(2) yes
O(5) Ni(1) O(3) 83.8(2) yes
O(13) S(1) O(12) 112.2(2) yes
O(12) S(1) O(11) 112.3(3) yes
O(12) S(1) C(110) 106.5(3) yes
C(110) C(11) C(12) 108.3(4) yes
C(110) C(11) C(17) 123.3(5) yes
O(14) C(12) C(13) 126.2(4) yes
C(11) C(110) S(1) 120.6(3) yes
O(22) S(2) O(21) 112.9(3) yes
O(22) S(2) C(210) 106.7(3) yes
O(21) S(2) C(210) 104.9(2) yes
C(210) C(21) C(22) 110.5(4) yes
O(24) C(22) C(23) 127.2(5) yes
C(21) C(27) C(24) 94.1(4) yes
O(13) S(1) O(11) 112.9(3) yes
O(13) S(1) C(110) 108.4(3) yes
O(11) S(1) C(110) 103.9(2) yes
C(110) C(11) C(16) 116.9(5) yes
O(14) C(12) C(11) 126.6(4) yes
C(14) C(17) C(11) 93.4(4) yes
O(22) S(2) O(23) 111.6(2) yes
O(23) S(2) O(21) 112.9(3) yes
O(23) S(2) C(210) 107.3(3) yes
C(210) C(21) C(27) 118.6(6) yes
C(210) C(21) C(26) 119.3(4) yes
O(24) C(22) C(21) 126.6(5) yes
C(21) C(210) S(2) 118.6(3) yes
C(14) C(13) C(12) 101.2(3) no
C(15) C(14) C(17) 102.2(4) no
C(18) C(17) C(19) 109.2(5) no
C(18) C(17) C(11) 116.7(4) no
C(27) C(21) C(22) 100.0(4) no
C(22) C(21) C(26) 103.1(5) no
C(23) C(22) C(21) 106.2(4) no
C(23) C(24) C(27) 101.9(4) no
C(25) C(26) C(21) 104.2(4) no
C(28) C(27) C(21) 115.6(4) no
C(12) C(11) C(16) 102.5(4) no
C(16) C(11) C(17) 102.3(4) no
C(11) C(12) C(13) 107.1(4) no
C(13) C(14) C(17) 103.9(4) no
C(11) C(16) C(15) 104.2(4) no
C(19) C(17) C(14) 113.0(5) no
C(27) C(21) C(26) 102.7(4) no
C(23) C(24) C(25) 106.2(5) no
C(24) C(25) C(26) 103.0(3) no
C(29) C(27) C(21) 114.6(4) no
C(28) C(27) C(24) 112.8(4) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni(1) O(1) . . 2.050(5) yes
Ni(1) O(3) . . 2.073(5) yes
Ni(1) O(5) . . 2.056(5) yes
Ni(1) O(2) . . 2.029(3) yes
Ni(1) O(4) . . 2.041(3) yes
Ni(1) O(6) . . 2.058(5) yes
S(1) O(11) . . 1.467(3) yes
S(1) O(13) . . 1.463(5) yes
O(14) C(12) . . 1.214(6) yes
S(2) O(22) . . 1.462(5) yes
S(2) C(210) . . 1.776(4) yes
S(1) O(12) . . 1.466(5) yes
S(1) C(110) . . 1.776(4) yes
S(2) O(21) . . 1.467(3) yes
S(2) O(23) . . 1.464(5) yes
O(24) C(22) . . 1.199(7) yes
O(1) H(11) . . 0.87(2) no
O(2) H(22) . . 0.87(2) no
O(4) H(41) . . 0.86(2) no
O(5) H(52) . . 0.85(2) no
C(11) C(12) . . 1.530(6) no
C(12) C(13) . . 1.530(6) no
C(14) C(17) . . 1.559(7) no
C(17) C(19) . . 1.537(7) no
C(21) C(210) . . 1.534(5) no
C(21) C(26) . . 1.566(6) no
C(24) C(25) . . 1.543(7) no
C(27) C(29) . . 1.521(8) no
O(1) H(12) . . 0.86(2) no
O(3) H(31) . . 0.87(2) no
O(4) H(42) . . 0.86(2) no
O(6) H(61) . . 0.86(2) no
C(11) C(16) . . 1.551(9) no
C(13) C(14) . . 1.529(6) no
C(15) C(16) . . 1.554(6) no
C(21) C(27) . . 1.552(8) no
C(22) C(23) . . 1.525(7) no
C(24) C(27) . . 1.568(6) no
C(27) C(28) . . 1.534(7) no
O(2) H(21) . . 0.88(2) no
O(3) H(32) . . 0.87(2) no
O(5) H(51) . . 0.86(2) no
O(6) H(62) . . 0.86(2) no
C(11) C(110) . . 1.525(5) no
C(11) C(17) . . 1.573(6) no
C(14) C(15) . . 1.554(9) no
C(17) C(18) . . 1.531(6) no
C(21) C(22) . . 1.545(8) no
C(23) C(24) . . 1.541(7) no
C(25) C(26) . . 1.553(6) no
