#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/03/7010377.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_7010377
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            'C26 H36 Ni O6 Rb S10'
_chemical_formula_weight         909.33
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.999(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.706(3)
_cell_length_b                   10.846(3)
_cell_length_c                   16.196(4)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     1798.5(9)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_method       Omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3245
_diffrn_reflns_theta_full        70.19
_diffrn_reflns_theta_max         70.19
_diffrn_reflns_theta_min         4.43
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.168
_exptl_absorpt_correction_T_max  0.291
_exptl_absorpt_correction_T_min  0.109
_exptl_absorpt_correction_type   'Optimised numerical'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.43
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1027P)²+0.3821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                2885
_reflns_number_total             3234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008299f.txt
_cod_data_source_block           nrrbo1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1798.4(7)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7010377
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
Ni1 Ni 0.0000 0.0000 0.5000 0.0270(2) Uani 1 2 d S . .
S1 S 0.13156(8) -0.10588(7) 0.44829(5) 0.0345(2) Uani 1 1 d . . .
C2 C 0.1505(3) -0.0099(3) 0.3685(2) 0.0307(7) Uani 1 1 d . . .
S3 S 0.24409(8) -0.04813(8) 0.29960(5) 0.0403(2) Uani 1 1 d . . .
C4 C 0.2161(3) 0.0862(3) 0.2386(2) 0.0377(7) Uani 1 1 d . . .
S4 S 0.27955(10) 0.11521(11) 0.15908(6) 0.0541(3) Uani 1 1 d . . .
S5 S 0.11444(8) 0.18812(8) 0.26943(5) 0.0382(2) Uani 1 1 d . . .
C6 C 0.0887(3) 0.1007(3) 0.35296(19) 0.0305(6) Uani 1 1 d . . .
S7 S -0.01233(7) 0.14896(6) 0.41091(5) 0.0309(2) Uani 1 1 d . . .
Rb1 Rb 1.0000 0.0000 0.0000 0.0513(2) Uani 1 2 d S . .
C1C C 0.9886(3) 0.3250(3) -0.0343(2) 0.0382(7) Uani 1 1 d . . .
H1C1 H 1.0604 0.3289 0.0204 0.046 Uiso 1 1 calc R . .
H1C2 H 0.9491 0.4081 -0.0463 0.046 Uiso 1 1 calc R . .
O2C O 0.8928(2) 0.2390(2) -0.02626(15) 0.0345(5) Uani 1 1 d . . .
C3C C 0.8370(3) 0.2715(3) 0.0404(2) 0.0374(7) Uani 1 1 d . . .
H3C1 H 0.7936 0.3528 0.0277 0.045 Uiso 1 1 calc R . .
H3C2 H 0.9064 0.2775 0.0962 0.045 Uiso 1 1 calc R . .
C4C C 0.7390(3) 0.1751(3) 0.0464(2) 0.0373(7) Uani 1 1 d . . .
H4C1 H 0.6821 0.2079 0.0796 0.045 Uiso 1 1 calc R . .
H4C2 H 0.6834 0.1537 -0.0122 0.045 Uiso 1 1 calc R . .
O5C O 0.8052(2) 0.0675(2) 0.08795(14) 0.0341(5) Uani 1 1 d . . .
C6C C 0.7185(3) -0.0355(3) 0.0835(2) 0.0329(7) Uani 1 1 d . . .
H6C H 0.6769 -0.0574 0.0216 0.039 Uiso 1 1 calc R . .
C7C C 0.6112(3) -0.0088(3) 0.1262(2) 0.0378(7) Uani 1 1 d . . .
H7C1 H 0.5604 0.0640 0.0983 0.045 Uiso 1 1 calc R . .
H7C2 H 0.5509 -0.0800 0.1173 0.045 Uiso 1 1 calc R . .
C8C C 0.6677(4) 0.0154(3) 0.2227(2) 0.0447(8) Uani 1 1 d . . .
H8C1 H 0.7203 0.0920 0.2318 0.054 Uiso 1 1 calc R . .
H8C2 H 0.5956 0.0270 0.2488 0.054 Uiso 1 1 calc R . .
C9C C 0.7529(4) -0.0919(3) 0.2665(2) 0.0449(8) Uani 1 1 d . . .
H9C1 H 0.6980 -0.1663 0.2627 0.054 Uiso 1 1 calc R . .
H9C2 H 0.7926 -0.0724 0.3283 0.054 Uiso 1 1 calc R . .
C10C C 0.8605(3) -0.1186(3) 0.2251(2) 0.0388(7) Uani 1 1 d . . .
H10A H 0.9117 -0.1911 0.2532 0.047 Uiso 1 1 calc R . .
H10B H 0.9203 -0.0471 0.2329 0.047 Uiso 1 1 calc R . .
C11C C 0.7999(3) -0.1441(3) 0.12896(19) 0.0317(6) Uani 1 1 d . . .
H11C H 0.7410 -0.2172 0.1229 0.038 Uiso 1 1 calc R . .
O12C O 0.8947(2) -0.1705(2) 0.08541(14) 0.0339(5) Uani 1 1 d . . .
C13C C 0.9583(3) -0.2868(3) 0.1063(2) 0.0398(7) Uani 1 1 d . . .
H13A H 0.8954 -0.3492 0.1143 0.048 Uiso 1 1 calc R . .
H13B H 1.0303 -0.2801 0.1608 0.048 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
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.4688 1.6079 '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
S7 Ni1 S7 180.0 . 3_556 ?
S7 Ni1 S1 93.34(3) . . ?
S7 Ni1 S1 86.66(3) 3_556 . ?
S7 Ni1 S1 86.66(3) . 3_556 ?
S7 Ni1 S1 93.34(3) 3_556 3_556 ?
S1 Ni1 S1 180.00(3) . 3_556 ?
C2 S1 Ni1 101.71(11) . . ?
C6 C2 S1 121.1(3) . . ?
C6 C2 S3 115.4(2) . . ?
S1 C2 S3 123.44(18) . . ?
C4 S3 C2 97.37(16) . . ?
S4 C4 S5 122.8(2) . . ?
S4 C4 S3 124.1(2) . . ?
S5 C4 S3 113.05(19) . . ?
C4 S4 Rb1 92.71(12) . 1_455 ?
C4 S5 C6 97.64(16) . . ?
C2 C6 S7 121.4(2) . . ?
C2 C6 S5 116.5(2) . . ?
S7 C6 S5 122.03(18) . . ?
C6 S7 Ni1 102.39(11) . . ?
O12C Rb1 O12C 180.00(11) 3_755 . ?
O12C Rb1 O2C 119.18(6) 3_755 3_755 ?
O12C Rb1 O2C 60.82(6) . 3_755 ?
O12C Rb1 O2C 60.82(6) 3_755 . ?
O12C Rb1 O2C 119.18(6) . . ?
O2C Rb1 O2C 180.00(9) 3_755 . ?
O12C Rb1 O5C 57.94(6) 3_755 3_755 ?
O12C Rb1 O5C 122.06(6) . 3_755 ?
O2C Rb1 O5C 61.89(6) 3_755 3_755 ?
O2C Rb1 O5C 118.11(6) . 3_755 ?
O12C Rb1 O5C 122.06(6) 3_755 . ?
O12C Rb1 O5C 57.94(6) . . ?
O2C Rb1 O5C 118.11(6) 3_755 . ?
O2C Rb1 O5C 61.89(6) . . ?
O5C Rb1 O5C 180.00(7) 3_755 . ?
O12C Rb1 S4 104.75(5) 3_755 3_655 ?
O12C Rb1 S4 75.25(5) . 3_655 ?
O2C Rb1 S4 90.31(5) 3_755 3_655 ?
O2C Rb1 S4 89.69(5) . 3_655 ?
O5C Rb1 S4 97.31(5) 3_755 3_655 ?
O5C Rb1 S4 82.69(5) . 3_655 ?
O12C Rb1 S4 75.25(5) 3_755 1_655 ?
O12C Rb1 S4 104.75(5) . 1_655 ?
O2C Rb1 S4 89.69(5) 3_755 1_655 ?
O2C Rb1 S4 90.31(5) . 1_655 ?
O5C Rb1 S4 82.69(5) 3_755 1_655 ?
O5C Rb1 S4 97.31(5) . 1_655 ?
S4 Rb1 S4 180.00(3) 3_655 1_655 ?
O12C Rb1 C1C 41.81(7) 3_755 . ?
O12C Rb1 C1C 138.19(7) . . ?
O2C Rb1 C1C 158.05(7) 3_755 . ?
O2C Rb1 C1C 21.95(7) . . ?
O5C Rb1 C1C 99.63(7) 3_755 . ?
O5C Rb1 C1C 80.37(7) . . ?
S4 Rb1 C1C 104.55(6) 3_655 . ?
S4 Rb1 C1C 75.45(6) 1_655 . ?
O12C Rb1 C1C 138.19(7) 3_755 3_755 ?
O12C Rb1 C1C 41.81(7) . 3_755 ?
O2C Rb1 C1C 21.95(7) 3_755 3_755 ?
O2C Rb1 C1C 158.05(7) . 3_755 ?
O5C Rb1 C1C 80.37(7) 3_755 3_755 ?
O5C Rb1 C1C 99.63(7) . 3_755 ?
S4 Rb1 C1C 75.45(6) 3_655 3_755 ?
S4 Rb1 C1C 104.55(6) 1_655 3_755 ?
C1C Rb1 C1C 180.0 . 3_755 ?
O12C Rb1 C3C 99.69(7) 3_755 3_755 ?
O12C Rb1 C3C 80.31(7) . 3_755 ?
O2C Rb1 C3C 21.80(7) 3_755 3_755 ?
O2C Rb1 C3C 158.20(7) . 3_755 ?
O5C Rb1 C3C 41.76(7) 3_755 3_755 ?
O5C Rb1 C3C 138.24(7) . 3_755 ?
S4 Rb1 C3C 86.01(6) 3_655 3_755 ?
S4 Rb1 C3C 93.99(6) 1_655 3_755 ?
C1C Rb1 C3C 141.36(8) . 3_755 ?
C1C Rb1 C3C 38.64(8) 3_755 3_755 ?
O12C Rb1 C3C 80.31(7) 3_755 . ?
O12C Rb1 C3C 99.69(7) . . ?
O2C Rb1 C3C 158.20(7) 3_755 . ?
O2C Rb1 C3C 21.80(7) . . ?
O5C Rb1 C3C 138.24(7) 3_755 . ?
O5C Rb1 C3C 41.76(7) . . ?
S4 Rb1 C3C 93.99(6) 3_655 . ?
S4 Rb1 C3C 86.01(6) 1_655 . ?
C1C Rb1 C3C 38.64(8) . . ?
C1C Rb1 C3C 141.36(8) 3_755 . ?
C3C Rb1 C3C 180.00(12) 3_755 . ?
O2C C1C C13C 109.8(3) . 3_755 ?
O2C C1C Rb1 47.86(13) . . ?
C13C C1C Rb1 81.02(18) 3_755 . ?
C1C O2C C3C 112.5(2) . . ?
C1C O2C Rb1 110.19(17) . . ?
C3C O2C Rb1 110.87(18) . . ?
O2C C3C C4C 109.4(3) . . ?
O2C C3C Rb1 47.32(14) . . ?
C4C C3C Rb1 80.00(18) . . ?
O5C C4C C3C 109.8(3) . . ?
O5C C4C Rb1 50.56(14) . . ?
C3C C4C Rb1 75.95(18) . . ?
C4C O5C C6C 112.7(2) . . ?
C4C O5C Rb1 107.43(18) . . ?
C6C O5C Rb1 108.69(17) . . ?
O5C C6C C11C 107.8(2) . . ?
O5C C6C C7C 112.8(3) . . ?
C11C C6C C7C 109.1(3) . . ?
O5C C6C Rb1 49.45(14) . . ?
C11C C6C Rb1 80.99(17) . . ?
C7C C6C Rb1 162.3(2) . . ?
C8C C7C C6C 111.8(3) . . ?
C9C C8C C7C 110.5(3) . . ?
C8C C9C C10C 111.7(3) . . ?
C9C C10C C11C 109.4(3) . . ?
O12C C11C C6C 107.9(3) . . ?
O12C C11C C10C 112.9(2) . . ?
C6C C11C C10C 111.5(3) . . ?
O12C C11C Rb1 36.93(13) . . ?
C6C C11C Rb1 75.36(17) . . ?
C10C C11C Rb1 110.58(18) . . ?
C11C O12C C13C 114.9(2) . . ?
C11C O12C Rb1 124.88(18) . . ?
C13C O12C Rb1 118.53(18) . . ?
O12C C13C C1C 108.9(3) . 3_755 ?
O12C C13C Rb1 41.37(14) . . ?
C1C C13C Rb1 75.05(17) 3_755 . ?
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 S7 2.1444(8) . ?
Ni1 S7 2.1444(8) 3_556 ?
Ni1 S1 2.1665(8) . ?
Ni1 S1 2.1665(8) 3_556 ?
S1 C2 1.717(3) . ?
C2 C6 1.358(4) . ?
C2 S3 1.754(3) . ?
S3 C4 1.737(4) . ?
C4 S4 1.652(3) . ?
C4 S5 1.724(4) . ?
S4 Rb1 3.5564(13) 1_455 ?
S5 C6 1.739(3) . ?
C6 S7 1.708(3) . ?
Rb1 O12C 2.742(2) 3_755 ?
Rb1 O12C 2.742(2) . ?
Rb1 O2C 2.816(2) 3_755 ?
Rb1 O2C 2.816(2) . ?
Rb1 O5C 2.941(2) 3_755 ?
Rb1 O5C 2.941(2) . ?
Rb1 S4 3.5564(13) 3_655 ?
Rb1 S4 3.5564(13) 1_655 ?
Rb1 C1C 3.565(3) . ?
Rb1 C1C 3.565(3) 3_755 ?
Rb1 C3C 3.579(3) 3_755 ?
Rb1 C3C 3.579(3) . ?
C1C O2C 1.420(4) . ?
C1C C13C 1.496(5) 3_755 ?
O2C C3C 1.423(4) . ?
C3C C4C 1.504(5) . ?
C4C O5C 1.427(4) . ?
O5C C6C 1.441(4) . ?
C6C C11C 1.521(4) . ?
C6C C7C 1.531(5) . ?
C7C C8C 1.525(5) . ?
C8C C9C 1.520(5) . ?
C9C C10C 1.520(5) . ?
C10C C11C 1.527(4) . ?
C11C O12C 1.424(4) . ?
O12C C13C 1.426(4) . ?
C13C C1C 1.496(5) 3_755 ?
