#------------------------------------------------------------------------------
#$Date: 2022-05-06 18:41:55 +0200 (vie 06 de may de 2022) $
#$Revision: 275119 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/17/7011790.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_7011790
loop_
_publ_author_name
'Bobicz, Dorota'
'Kristiansson, Olof'
'Persson, Ingmar'
_publ_section_title
;
 Reactivity of five- and six-coordinated solvates. A complex formation
 and crystallographic study of the nickel(II) bromide and iodide
 systems in dimethyl sulfoxide and N,N'-dimethylpropyleneurea
;
_journal_coden_ASTM              JCSDAA
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4201
_journal_page_last               4205
_journal_paper_doi               10.1039/b204128f
_journal_year                    2002
_chemical_formula_sum            'C16 H48 Cl2 Ni O8 S8'
_chemical_formula_weight         754.63
_chemical_name_systematic
; 
hexakis(dimethylsulfoxide)nickel(II) chloride
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.208(4)
_cell_angle_beta                 66.751(3)
_cell_angle_gamma                87.620(3)
_cell_formula_units_Z            1
_cell_length_a                   9.9520(16)
_cell_length_b                   10.2209(16)
_cell_length_c                   11.0282(18)
_cell_measurement_reflns_used    12015
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.50
_cell_volume                     916.4(3)
_computing_cell_refinement       'Bruker SMART and SAINT (1998b)'
_computing_data_collection       'Bruker SMART (1998b)'
_computing_data_reduction        'Bruker SAINT (1998b)'
_computing_molecular_graphics    'Bruker SHELXTL (1998a)'
_computing_publication_material  'Bruker SHELXTL (1998a)'
_computing_structure_refinement  'Bruker SHELXTL (1998a)'
_computing_structure_solution    'Bruker SHELXTL (1998a)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.786
_diffrn_measured_fraction_theta_max 0.786
_diffrn_measurement_device_type
;
Bruker SMART diffractometer with CCD area detector 
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3807
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%
;
Neglible as determined from a repetition of the first 50
frames at the end of the experiment
;
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.8007
_exptl_absorpt_correction_T_min  0.6864
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_meas      1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.043(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0485
_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)+(0.0634P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                1895
_reflns_number_total             3140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204128f.txt
_cod_data_source_block           hexakis(dimethylsulfoxide)nickel(II)chloride
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7011790
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.5000 0.5000 0.0000 0.0357(3) Uani 1 2 d S . .
Cl1 Cl 0.22194(16) 0.81565(15) 0.44955(16) 0.0755(4) Uani 1 1 d . . .
S11 S 0.63769(13) 0.30313(12) 0.21153(14) 0.0469(3) Uani 1 1 d . . .
S21 S 0.28133(12) 0.22404(11) 0.26328(13) 0.0469(3) Uani 1 1 d . . .
S31 S 0.45591(12) 0.67539(12) 0.18127(14) 0.0471(3) Uani 1 1 d . . .
S41 S -0.04123(18) 0.74770(17) 0.2065(2) 0.0851(5) Uani 1 1 d . . .
O11 O 0.6278(3) 0.3404(3) 0.0671(3) 0.0448(8) Uani 1 1 d . . .
O21 O 0.3159(3) 0.3898(3) 0.1986(3) 0.0460(8) Uani 1 1 d . . .
O31 O 0.5662(3) 0.6154(3) 0.0837(3) 0.0453(8) Uani 1 1 d . . .
O41 O -0.0695(6) 0.7495(5) 0.0894(6) 0.1220(17) Uani 1 1 d . . .
C11 C 0.6738(8) 0.1207(5) 0.2764(7) 0.089(2) Uani 1 1 d . . .
H11A H 0.5882 0.0552 0.3058 0.134 Uiso 1 1 calc R . .
H11B H 0.6967 0.0958 0.3600 0.134 Uiso 1 1 calc R . .
H11C H 0.7564 0.1119 0.1988 0.134 Uiso 1 1 calc R . .
C12 C 0.8127(5) 0.3918(6) 0.1632(6) 0.0700(15) Uani 1 1 d . . .
H12A H 0.8129 0.4961 0.1243 0.105 Uiso 1 1 calc R . .
H12B H 0.8876 0.3711 0.0894 0.105 Uiso 1 1 calc R . .
H12C H 0.8326 0.3566 0.2496 0.105 Uiso 1 1 calc R . .
C21 C 0.1850(6) 0.1664(5) 0.4561(5) 0.0676(15) Uani 1 1 d . . .
H21A H 0.2527 0.1789 0.4941 0.101 Uiso 1 1 calc R . .
H21B H 0.1422 0.0646 0.5056 0.101 Uiso 1 1 calc R . .
H21C H 0.1080 0.2245 0.4732 0.101 Uiso 1 1 calc R . .
C22 C 0.1301(5) 0.1875(5) 0.2315(6) 0.0662(15) Uani 1 1 d . . .
H22A H 0.1627 0.2136 0.1285 0.099 Uiso 1 1 calc R . .
H22B H 0.0552 0.2445 0.2586 0.099 Uiso 1 1 calc R . .
H22C H 0.0899 0.0848 0.2903 0.099 Uiso 1 1 calc R . .
C31 C 0.5583(6) 0.8343(6) 0.1416(9) 0.121(3) Uani 1 1 d . . .
H31A H 0.5733 0.9096 0.0449 0.181 Uiso 1 1 calc R . .
H31B H 0.6525 0.8134 0.1438 0.181 Uiso 1 1 calc R . .
H31C H 0.5055 0.8674 0.2142 0.181 Uiso 1 1 calc R . .
C32 C 0.4444(9) 0.5665(7) 0.3585(7) 0.128(3) Uani 1 1 d . . .
H32A H 0.3918 0.4703 0.3974 0.192 Uiso 1 1 calc R . .
H32B H 0.3926 0.6105 0.4215 0.192 Uiso 1 1 calc R . .
H32C H 0.5423 0.5583 0.3545 0.192 Uiso 1 1 calc R . .
C41 C 0.1201(7) 0.8725(6) 0.1291(7) 0.0875(19) Uani 1 1 d . . .
H41A H 0.1034 0.9705 0.0773 0.131 Uiso 1 1 calc R . .
H41B H 0.1997 0.8488 0.0611 0.131 Uiso 1 1 calc R . .
H41C H 0.1456 0.8664 0.2066 0.131 Uiso 1 1 calc R . .
C42 C 0.0290(7) 0.5859(5) 0.2886(7) 0.0829(18) Uani 1 1 d . . .
H42A H -0.0471 0.5021 0.3398 0.124 Uiso 1 1 calc R . .
H42B H 0.0605 0.5933 0.3575 0.124 Uiso 1 1 calc R . .
H42C H 0.1117 0.5748 0.2127 0.124 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 0.0033 0.0016 '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 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
O31 Ni1 O31 180.00(11) 2_665 . ?
O31 Ni1 O21 89.19(11) 2_665 . ?
O31 Ni1 O21 90.81(11) . . ?
O31 Ni1 O11 90.06(11) 2_665 2_665 ?
O31 Ni1 O11 89.94(11) . 2_665 ?
O21 Ni1 O11 87.87(11) . 2_665 ?
O21 Ni1 O11 92.13(11) 2_665 2_665 ?
O31 Ni1 O11 89.94(11) 2_665 . ?
O31 Ni1 O11 90.06(11) . . ?
O21 Ni1 O11 92.13(11) . . ?
O11 S11 C11 105.6(2) . . ?
O11 S11 C12 106.2(2) . . ?
C11 S11 C12 98.0(3) . . ?
O21 S21 C22 106.9(2) . . ?
O21 S21 C21 103.1(2) . . ?
C22 S21 C21 97.7(2) . . ?
O31 S31 C32 105.3(2) . . ?
O31 S31 C31 103.6(2) . . ?
C32 S31 C31 98.3(4) . . ?
O41 S41 C41 108.4(3) . . ?
O41 S41 C42 110.9(3) . . ?
C41 S41 C42 97.0(3) . . ?
S11 O11 Ni1 117.89(15) . . ?
S21 O21 Ni1 117.90(16) . . ?
S31 O31 Ni1 121.69(15) . . ?
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 O31 2.041(3) . ?
Ni1 O21 2.069(3) . ?
Ni1 O11 2.085(3) . ?
S11 O11 1.511(3) . ?
S11 C11 1.762(5) . ?
S11 C12 1.765(5) . ?
S21 O21 1.517(3) . ?
S21 C22 1.762(5) . ?
S21 C21 1.771(5) . ?
S31 O31 1.525(3) . ?
S31 C32 1.735(6) . ?
S31 C31 1.742(5) . ?
S41 O41 1.418(5) . ?
S41 C41 1.753(6) . ?
S41 C42 1.773(5) . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2022-05-06T19:40:00+03:00
'Updated bibliographic information.'
