#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/03/7010376.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_7010376
loop_
_publ_author_name
'Cronin, Leroy'
'Clark, Stewart J.'
'Parsons, Simon'
'Nakamura, Takayoshi'
'Robertson, Neil'
_publ_section_title
;
 Unique structural topologies involving metal--metal and metal--sulfur
 interactions: salts of [Ni(C3S5)2]x− with
 cis-anti-cis-dicyclohexyl-18-crown-6 complexed counter ions
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1347
_journal_paper_doi               10.1039/b008299f
_journal_year                    2001
_chemical_formula_sum            'C46 H72 Ni O12 Rb2 S10'
_chemical_formula_weight         1367.29
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.71(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.636(7)
_cell_length_b                   8.484(6)
_cell_length_c                   24.440(7)
_cell_measurement_temperature    293(2)
_cell_volume                     3025(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            6966
_diffrn_reflns_theta_full        27.66
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    2.318
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+1.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                4187
_reflns_number_total             6966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008299f.txt
_cod_data_source_block           rb-cath
_cod_original_cell_volume        3024(3)
_cod_database_code               7010376
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb Rb 0.10882(3) 1.06337(5) 0.135707(17) 0.05700(14) Uani 1 1 d . . .
Ni Ni 0.0000 1.0000 0.0000 0.0528(2) Uani 1 2 d S . .
S1 S -0.41745(11) 0.9243(3) 0.12983(7) 0.1083(6) Uani 1 1 d . . .
S2 S -0.23140(9) 0.81383(18) 0.10925(5) 0.0792(4) Uani 1 1 d . . .
S3 S -0.29543(9) 1.10486(17) 0.06068(6) 0.0765(4) Uani 1 1 d . . .
S4 S -0.05173(8) 0.82690(15) 0.05555(5) 0.0696(3) Uani 1 1 d . . .
S5 S -0.12409(8) 1.14550(14) -0.00105(5) 0.0653(3) Uani 1 1 d . . .
O1 O -0.0287(2) 1.0919(4) 0.22118(13) 0.0646(8) Uani 1 1 d . . .
O2 O 0.1203(2) 0.8994(4) 0.24252(13) 0.0649(8) Uani 1 1 d . . .
O3 O 0.26870(19) 0.8974(4) 0.17955(12) 0.0631(7) Uani 1 1 d . . .
O4 O 0.3106(2) 1.1555(3) 0.10839(11) 0.0583(7) Uani 1 1 d . . .
O5 O 0.1658(2) 1.3593(3) 0.09372(13) 0.0674(8) Uani 1 1 d . . .
O6 O 0.0123(2) 1.3585(4) 0.15519(13) 0.0678(8) Uani 1 1 d . . .
C1 C -0.3200(3) 0.9470(7) 0.1015(2) 0.0746(13) Uani 1 1 d . . .
C2 C -0.1559(3) 0.9087(5) 0.06832(18) 0.0597(11) Uani 1 1 d . . .
C3 C -0.1872(3) 1.0438(5) 0.04477(18) 0.0580(10) Uani 1 1 d . . .
C4 C -0.1659(4) 0.8760(8) 0.2633(2) 0.0912(17) Uani 1 1 d . . .
H4A H -0.2206 0.8522 0.2817 0.109 Uiso 1 1 calc R . .
H4B H -0.1846 0.9312 0.2294 0.109 Uiso 1 1 calc R . .
C5 C -0.1179(4) 0.7239(7) 0.2502(3) 0.0936(17) Uani 1 1 d . . .
H5A H -0.1573 0.6635 0.2242 0.112 Uiso 1 1 calc R . .
H5B H -0.1077 0.6619 0.2835 0.112 Uiso 1 1 calc R . .
C6 C -0.0253(3) 0.7532(6) 0.2262(2) 0.0737(13) Uani 1 1 d . . .
H6A H 0.0059 0.6536 0.2222 0.088 Uiso 1 1 calc R . .
H6B H -0.0359 0.8006 0.1901 0.088 Uiso 1 1 calc R . .
C7 C 0.0343(3) 0.8616(5) 0.26340(18) 0.0612(10) Uani 1 1 d . . .
H7 H 0.0471 0.8083 0.2988 0.073 Uiso 1 1 calc R . .
C8 C 0.1838(3) 0.7745(6) 0.2463(2) 0.0718(12) Uani 1 1 d . . .
H8A H 0.1630 0.6913 0.2211 0.086 Uiso 1 1 calc R . .
H8B H 0.1879 0.7316 0.2833 0.086 Uiso 1 1 calc R . .
C9 C 0.2760(3) 0.8306(6) 0.23295(19) 0.0655(11) Uani 1 1 d . . .
H9A H 0.2989 0.9089 0.2596 0.079 Uiso 1 1 calc R . .
H9B H 0.3188 0.7430 0.2344 0.079 Uiso 1 1 calc R . .
C10 C 0.3551(3) 0.9241(5) 0.15843(19) 0.0605(11) Uani 1 1 d . . .
H10A H 0.3873 0.8248 0.1558 0.073 Uiso 1 1 calc R . .
H10B H 0.3920 0.9928 0.1830 0.073 Uiso 1 1 calc R . .
C11 C 0.3407(3) 0.9983(5) 0.10285(18) 0.0624(11) Uani 1 1 d . . .
H11A H 0.3976 0.9971 0.0851 0.075 Uiso 1 1 calc R . .
H11B H 0.2952 0.9391 0.0802 0.075 Uiso 1 1 calc R . .
C12 C 0.2922(3) 1.2360(6) 0.05653(17) 0.0640(11) Uani 1 1 d . . .
H12 H 0.2497 1.1721 0.0327 0.077 Uiso 1 1 calc R . .
C13 C 0.3795(4) 1.2649(7) 0.02729(19) 0.0802(14) Uani 1 1 d . . .
H13A H 0.4098 1.1652 0.0218 0.096 Uiso 1 1 calc R . .
H13B H 0.3632 1.3113 -0.0085 0.096 Uiso 1 1 calc R . .
C14 C 0.4450(4) 1.3746(7) 0.0607(2) 0.0864(16) Uani 1 1 d . . .
H14A H 0.4652 1.3246 0.0953 0.104 Uiso 1 1 calc R . .
H14B H 0.4986 1.3939 0.0408 0.104 Uiso 1 1 calc R . .
C15 C 0.3992(4) 1.5292(7) 0.0717(2) 0.0891(17) Uani 1 1 d . . .
H15A H 0.3846 1.5841 0.0373 0.107 Uiso 1 1 calc R . .
H15B H 0.4411 1.5947 0.0946 0.107 Uiso 1 1 calc R . .
C16 C 0.3116(4) 1.5034(6) 0.1004(2) 0.0733(13) Uani 1 1 d . . .
H16A H 0.3270 1.4602 0.1367 0.088 Uiso 1 1 calc R . .
H16B H 0.2811 1.6037 0.1045 0.088 Uiso 1 1 calc R . .
C17 C 0.2469(3) 1.3914(5) 0.06768(18) 0.0649(11) Uani 1 1 d . . .
H17 H 0.2289 1.4410 0.0322 0.078 Uiso 1 1 calc R . .
C18 C 0.1034(4) 1.4882(6) 0.0933(3) 0.0872(16) Uani 1 1 d . . .
H18A H 0.1016 1.5420 0.0582 0.105 Uiso 1 1 calc R . .
H18B H 0.1236 1.5628 0.1218 0.105 Uiso 1 1 calc R . .
C19 C 0.0105(4) 1.4282(6) 0.1028(2) 0.0812(15) Uani 1 1 d . . .
H19A H -0.0332 1.5144 0.1002 0.097 Uiso 1 1 calc R . .
H19B H -0.0088 1.3509 0.0749 0.097 Uiso 1 1 calc R . .
C20 C -0.0767(3) 1.3129(6) 0.1681(2) 0.0789(14) Uani 1 1 d . . .
H20A H -0.1022 1.2369 0.1414 0.095 Uiso 1 1 calc R . .
H20B H -0.1167 1.4041 0.1671 0.095 Uiso 1 1 calc R . .
C21 C -0.0704(4) 1.2420(6) 0.2238(2) 0.0814(15) Uani 1 1 d . . .
H21A H -0.0341 1.3092 0.2493 0.098 Uiso 1 1 calc R . .
H21B H -0.1311 1.2316 0.2365 0.098 Uiso 1 1 calc R . .
C22 C -0.0135(3) 1.0142(6) 0.27358(18) 0.0635(11) Uani 1 1 d . . .
H22 H 0.0264 1.0799 0.2984 0.076 Uiso 1 1 calc R . .
C23 C -0.1027(4) 0.9811(7) 0.2999(2) 0.0841(16) Uani 1 1 d . . .
H23A H -0.0888 0.9300 0.3351 0.101 Uiso 1 1 calc R . .
H23B H -0.1334 1.0799 0.3063 0.101 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rb Rb -0.9393 2.9676 '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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 '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'
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
O5 Rb O3 108.19(9) . . ?
O5 Rb O6 57.84(10) . . ?
O3 Rb O6 138.49(9) . . ?
O5 Rb O2 137.18(9) . . ?
O3 Rb O2 56.74(8) . . ?
O6 Rb O2 104.60(9) . . ?
O5 Rb O1 114.02(9) . . ?
O3 Rb O1 110.51(9) . . ?
O6 Rb O1 57.54(9) . . ?
O2 Rb O1 54.54(8) . . ?
O5 Rb O4 53.54(8) . . ?
O3 Rb O4 56.94(8) . . ?
O6 Rb O4 107.00(9) . . ?
O2 Rb O4 108.38(8) . . ?
O1 Rb O4 143.82(8) . . ?
O5 Rb C19 42.62(11) . . ?
O3 Rb C19 146.51(11) . . ?
O6 Rb C19 23.46(11) . . ?
O2 Rb C19 128.06(12) . . ?
O1 Rb C19 78.62(11) . . ?
O4 Rb C19 96.12(11) . . ?
O5 Rb S4 119.77(7) . . ?
O3 Rb S4 114.33(8) . . ?
O6 Rb S4 105.42(8) . . ?
O2 Rb S4 102.05(8) . . ?
O1 Rb S4 88.78(7) . . ?
O4 Rb S4 127.36(6) . . ?
C19 Rb S4 97.60(11) . . ?
O5 Rb C20 79.02(11) . . ?
O3 Rb C20 144.97(11) . . ?
O6 Rb C20 22.45(10) . . ?
O2 Rb C20 94.13(11) . . ?
O1 Rb C20 40.64(10) . . ?
O4 Rb C20 129.44(11) . . ?
C19 Rb C20 38.65(12) . . ?
S4 Rb C20 88.66(10) . . ?
O5 Rb C11 75.30(10) . . ?
O3 Rb C11 41.42(9) . . ?
O6 Rb C11 130.06(10) . . ?
O2 Rb C11 97.99(10) . . ?
O1 Rb C11 149.32(10) . . ?
O4 Rb C11 23.08(9) . . ?
C19 Rb C11 117.73(11) . . ?
S4 Rb C11 112.58(8) . . ?
C20 Rb C11 152.49(12) . . ?
O5 Rb Ni 85.45(7) . . ?
O3 Rb Ni 123.90(7) . . ?
O6 Rb Ni 95.42(7) . . ?
O2 Rb Ni 137.19(7) . . ?
O1 Rb Ni 112.26(7) . . ?
O4 Rb Ni 101.05(6) . . ?
C19 Rb Ni 77.07(10) . . ?
S4 Rb Ni 35.44(2) . . ?
C20 Rb Ni 90.34(10) . . ?
C11 Rb Ni 97.22(8) . . ?
O5 Rb C12 39.40(10) . . ?
O3 Rb C12 77.68(10) . . ?
O6 Rb C12 97.21(11) . . ?
O2 Rb C12 130.71(9) . . ?
O1 Rb C12 150.82(9) . . ?
O4 Rb C12 22.33(8) . . ?
C19 Rb C12 80.36(12) . . ?
S4 Rb C12 113.98(7) . . ?
C20 Rb C12 118.22(12) . . ?
C11 Rb C12 38.04(11) . . ?
Ni Rb C12 82.15(7) . . ?
S4 Ni S4 180.00(5) 3_575 . ?
S4 Ni S5 93.26(6) 3_575 3_575 ?
S4 Ni S5 86.74(6) . 3_575 ?
S4 Ni S5 86.74(6) 3_575 . ?
S4 Ni S5 93.26(6) . . ?
S5 Ni S5 180.00(3) 3_575 . ?
S4 Ni Rb 71.13(4) 3_575 3_575 ?
S4 Ni Rb 108.87(4) . 3_575 ?
S5 Ni Rb 103.30(4) 3_575 3_575 ?
S5 Ni Rb 76.70(4) . 3_575 ?
S4 Ni Rb 108.87(4) 3_575 . ?
S4 Ni Rb 71.13(4) . . ?
S5 Ni Rb 76.70(4) 3_575 . ?
S5 Ni Rb 103.30(4) . . ?
Rb Ni Rb 180.000(6) 3_575 . ?
C1 S2 C2 98.1(2) . . ?
C1 S3 C3 97.7(2) . . ?
C2 S4 Ni 101.46(16) . . ?
C2 S4 Rb 103.11(16) . . ?
Ni S4 Rb 73.44(5) . . ?
C3 S5 Ni 101.32(16) . . ?
C3 S5 Rb 113.76(15) . 3_575 ?
Ni S5 Rb 68.69(4) . 3_575 ?
C21 O1 C22 114.0(4) . . ?
C21 O1 Rb 114.6(3) . . ?
C22 O1 Rb 121.0(2) . . ?
C8 O2 C7 113.7(3) . . ?
C8 O2 Rb 113.8(2) . . ?
C7 O2 Rb 115.7(2) . . ?
C9 O3 C10 113.3(3) . . ?
C9 O3 Rb 122.6(2) . . ?
C10 O3 Rb 120.6(2) . . ?
C11 O4 C12 113.5(3) . . ?
C11 O4 Rb 95.2(2) . . ?
C12 O4 Rb 101.0(2) . . ?
C17 O5 C18 114.1(3) . . ?
C17 O5 Rb 127.5(3) . . ?
C18 O5 Rb 118.1(3) . . ?
C19 O6 C20 111.6(4) . . ?
C19 O6 Rb 100.6(3) . . ?
C20 O6 Rb 105.4(3) . . ?
S1 C1 S2 123.2(3) . . ?
S1 C1 S3 124.2(3) . . ?
S2 C1 S3 112.5(3) . . ?
C3 C2 S4 122.7(3) . . ?
C3 C2 S2 115.3(3) . . ?
S4 C2 S2 121.8(3) . . ?
C2 C3 S5 121.2(3) . . ?
C2 C3 S3 116.2(3) . . ?
S5 C3 S3 122.5(3) . . ?
C5 C4 C23 110.6(5) . . ?
C4 C5 C6 112.4(4) . . ?
C7 C6 C5 110.4(4) . . ?
O2 C7 C22 107.5(4) . . ?
O2 C7 C6 113.6(4) . . ?
C22 C7 C6 111.6(4) . . ?
O2 C8 C9 110.4(4) . . ?
O2 C8 Rb 46.11(19) . . ?
C9 C8 Rb 81.4(2) . . ?
O3 C9 C8 109.1(4) . . ?
O3 C10 C11 109.5(3) . . ?
O4 C11 C10 109.4(3) . . ?
O4 C11 Rb 61.74(19) . . ?
C10 C11 Rb 85.8(2) . . ?
O4 C12 C17 107.9(3) . . ?
O4 C12 C13 112.4(4) . . ?
C17 C12 C13 109.8(4) . . ?
O4 C12 Rb 56.66(19) . . ?
C17 C12 Rb 84.5(2) . . ?
C13 C12 Rb 164.9(3) . . ?
C14 C13 C12 111.1(4) . . ?
C15 C14 C13 110.9(5) . . ?
C14 C15 C16 111.1(4) . . ?
C17 C16 C15 111.1(4) . . ?
O5 C17 C12 108.0(3) . . ?
O5 C17 C16 113.1(4) . . ?
C12 C17 C16 112.2(4) . . ?
O5 C18 C19 109.3(4) . . ?
O5 C18 Rb 42.3(2) . . ?
C19 C18 Rb 68.1(2) . . ?
O6 C19 C18 109.6(4) . . ?
O6 C19 Rb 55.9(2) . . ?
C18 C19 Rb 88.5(3) . . ?
O6 C20 C21 109.0(4) . . ?
O6 C20 Rb 52.1(2) . . ?
C21 C20 Rb 88.4(3) . . ?
O1 C21 C20 108.6(4) . . ?
O1 C22 C7 106.7(3) . . ?
O1 C22 C23 112.6(4) . . ?
C7 C22 C23 109.7(4) . . ?
C4 C23 C22 111.1(4) . . ?
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
Rb O5 2.862(3) . ?
Rb O3 2.863(3) . ?
Rb O6 2.933(3) . ?
Rb O2 2.950(3) . ?
Rb O1 3.027(3) . ?
Rb O4 3.178(3) . ?
Rb C19 3.480(5) . ?
Rb S4 3.5538(19) . ?
Rb C20 3.582(5) . ?
Rb C11 3.593(5) . ?
Rb Ni 3.5999(12) . ?
Rb C12 3.734(5) . ?
Ni S4 2.1776(14) 3_575 ?
Ni S4 2.1776(14) . ?
Ni S5 2.1944(14) 3_575 ?
Ni S5 2.1944(14) . ?
Ni Rb 3.5999(12) 3_575 ?
S1 C1 1.647(5) . ?
S2 C1 1.719(6) . ?
S2 C2 1.747(4) . ?
S3 C1 1.725(6) . ?
S3 C3 1.741(4) . ?
S4 C2 1.727(5) . ?
S5 C3 1.738(4) . ?
S5 Rb 3.7605(17) 3_575 ?
O1 C21 1.416(6) . ?
O1 C22 1.441(5) . ?
O2 C8 1.408(5) . ?
O2 C7 1.433(5) . ?
O3 C9 1.419(5) . ?
O3 C10 1.422(5) . ?
O4 C11 1.414(5) . ?
O4 C12 1.445(5) . ?
O5 C17 1.418(5) . ?
O5 C18 1.424(6) . ?
O6 C19 1.409(6) . ?
O6 C20 1.419(6) . ?
C2 C3 1.346(6) . ?
C4 C5 1.515(8) . ?
C4 C23 1.522(8) . ?
C5 C6 1.541(7) . ?
C6 C7 1.518(6) . ?
C7 C22 1.503(7) . ?
C8 C9 1.493(6) . ?
C10 C11 1.497(6) . ?
C12 C17 1.510(7) . ?
C12 C13 1.534(6) . ?
C13 C14 1.525(7) . ?
C14 C15 1.507(8) . ?
C15 C16 1.527(7) . ?
C16 C17 1.521(6) . ?
C18 C19 1.489(7) . ?
C20 C21 1.483(7) . ?
C22 C23 1.527(6) . ?
