#------------------------------------------------------------------------------
#$Date: 2022-05-06 19:41:55 +0300 (Fri, 06 May 2022) $
#$Revision: 275119 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/17/7011791.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_7011791
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 Br2 Ni O8 S8'
_chemical_formula_weight         843.55
_chemical_name_systematic
; 
hexakis(dimethylsulfoxide)nickel(II) bromide
;
_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                63.608(12)
_cell_angle_beta                 67.713(8)
_cell_angle_gamma                87.889(9)
_cell_formula_units_Z            1
_cell_length_a                   9.900(5)
_cell_length_b                   10.380(6)
_cell_length_c                   11.295(6)
_cell_measurement_reflns_used    12015
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.50
_cell_volume                     949.8(9)
_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 0.740
_diffrn_measured_fraction_theta_max 0.740
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.1482
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3516
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%
;
Approximately 20 % as determined from a repetition of the first 50
frames at the end of the experiment
;
_exptl_absorpt_coefficient_mu    3.085
_exptl_absorpt_correction_T_max  0.5248
_exptl_absorpt_correction_T_min  0.3870
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.653
_refine_diff_density_min         -2.181
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.440
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.440
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.1100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2355
_refine_ls_wR_factor_ref         0.2433
_reflns_number_gt                1346
_reflns_number_total             3076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204128f.txt
_cod_data_source_block           hexakis(dimethylsulfoxide)nickel(II)bromide
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011791
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 0.5000 0.0500(9) Uani 1 2 d S . .
Br1 Br 0.23981(19) 0.8140(2) -0.0522(2) 0.0895(9) Uani 1 1 d . . .
S11 S 0.5296(4) 0.3307(4) 0.3247(4) 0.0613(12) Uani 1 1 d . . .
S21 S 0.7172(4) 0.7729(4) 0.2343(4) 0.0601(12) Uani 1 1 d . . .
S31 S 0.3580(4) 0.6994(4) 0.2971(4) 0.0570(12) Uani 1 1 d . . .
S41 S 0.0416(5) 0.2527(6) 0.2908(6) 0.0933(16) Uani 1 1 d . . .
O11 O 0.4224(8) 0.3870(9) 0.4226(10) 0.056(3) Uani 1 1 d . . .
O21 O 0.6862(9) 0.6084(11) 0.3041(10) 0.071(3) Uani 1 1 d . . .
O31 O 0.3745(9) 0.6598(9) 0.4345(10) 0.059(3) Uani 1 1 d . . .
O41 O 0.0684(13) 0.2483(15) 0.4103(15) 0.118(4) Uani 1 1 d . . .
C11 C 0.518(3) 0.428(2) 0.163(2) 0.136(8) Uani 1 1 d . . .
H11A H 0.5666 0.5266 0.1187 0.204 Uiso 1 1 calc R . .
H11B H 0.4155 0.4291 0.1782 0.204 Uiso 1 1 calc R . .
H11C H 0.5640 0.3850 0.1016 0.204 Uiso 1 1 calc R . .
C12 C 0.4304(19) 0.1599(18) 0.381(2) 0.108(7) Uani 1 1 d . . .
H12A H 0.4275 0.0906 0.4732 0.162 Uiso 1 1 calc R . .
H12B H 0.4789 0.1257 0.3111 0.162 Uiso 1 1 calc R . .
H12C H 0.3314 0.1712 0.3877 0.162 Uiso 1 1 calc R . .
C21 C 0.8056(17) 0.8286(19) 0.0490(16) 0.099(6) Uani 1 1 d . . .
H21A H 0.7354 0.8137 0.0147 0.149 Uiso 1 1 calc R . .
H21B H 0.8834 0.7727 0.0317 0.149 Uiso 1 1 calc R . .
H21C H 0.8467 0.9301 -0.0012 0.149 Uiso 1 1 calc R . .
C22 C 0.8702(16) 0.8127(17) 0.2648(18) 0.077(5) Uani 1 1 d . . .
H22A H 0.8389 0.7868 0.3651 0.116 Uiso 1 1 calc R . .
H22B H 0.9085 0.9149 0.2069 0.116 Uiso 1 1 calc R . .
H22C H 0.9459 0.7579 0.2389 0.116 Uiso 1 1 calc R . .
C31 C 0.1783(15) 0.6111(16) 0.3519(19) 0.085(5) Uani 1 1 d . . .
H31A H 0.1780 0.5080 0.3889 0.127 Uiso 1 1 calc R . .
H31B H 0.1521 0.6472 0.2705 0.127 Uiso 1 1 calc R . .
H31C H 0.1080 0.6303 0.4260 0.127 Uiso 1 1 calc R . .
C32 C 0.322(2) 0.8819(17) 0.2338(19) 0.095(6) Uani 1 1 d . . .
H32A H 0.4106 0.9466 0.2001 0.142 Uiso 1 1 calc R . .
H32B H 0.2451 0.8913 0.3111 0.142 Uiso 1 1 calc R . .
H32C H 0.2923 0.9065 0.1558 0.142 Uiso 1 1 calc R . .
C41 C -0.118(2) 0.129(2) 0.373(2) 0.140(9) Uani 1 1 d . . .
H41A H -0.0991 0.0326 0.4224 0.211 Uiso 1 1 calc R . .
H41B H -0.1497 0.1341 0.3003 0.211 Uiso 1 1 calc R . .
H41C H -0.1942 0.1521 0.4403 0.211 Uiso 1 1 calc R . .
C42 C -0.030(2) 0.414(2) 0.210(2) 0.137(9) Uani 1 1 d . . .
H42A H 0.0474 0.4962 0.1567 0.205 Uiso 1 1 calc R . .
H42B H -0.1092 0.4258 0.2835 0.205 Uiso 1 1 calc R . .
H42C H -0.0655 0.4053 0.1449 0.205 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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
O11 Ni1 O11 180.0(3) . 2_666 ?
O11 Ni1 O31 90.4(3) . 2_666 ?
O11 Ni1 O31 89.6(3) 2_666 2_666 ?
O11 Ni1 O31 89.6(3) . . ?
O11 Ni1 O31 90.4(3) 2_666 . ?
O31 Ni1 O31 180.0(6) 2_666 . ?
O11 Ni1 O21 92.2(4) . . ?
O11 Ni1 O21 87.8(4) 2_666 . ?
O31 Ni1 O21 87.3(4) 2_666 . ?
O31 Ni1 O21 92.7(4) . . ?
O11 Ni1 O21 87.8(4) . 2_666 ?
O11 Ni1 O21 92.2(4) 2_666 2_666 ?
O31 Ni1 O21 92.7(4) 2_666 2_666 ?
O31 Ni1 O21 87.3(4) . 2_666 ?
O21 Ni1 O21 180.000(1) . 2_666 ?
O11 S11 C11 104.1(8) . . ?
O11 S11 C12 103.2(7) . . ?
C11 S11 C12 99.4(10) . . ?
O21 S21 C21 104.7(7) . . ?
O21 S21 C22 105.1(6) . . ?
C21 S21 C22 99.1(7) . . ?
O31 S31 C31 105.0(7) . . ?
O31 S31 C32 106.3(7) . . ?
C31 S31 C32 98.2(8) . . ?
O41 S41 C41 104.5(9) . . ?
O41 S41 C42 110.7(10) . . ?
C41 S41 C42 98.0(9) . . ?
S11 O11 Ni1 120.3(4) . . ?
S21 O21 Ni1 117.7(6) . . ?
S31 O31 Ni1 119.1(5) . . ?
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 O11 2.054(9) . ?
Ni1 O11 2.054(9) 2_666 ?
Ni1 O31 2.073(8) 2_666 ?
Ni1 O31 2.073(8) . ?
Ni1 O21 2.099(9) . ?
Ni1 O21 2.099(9) 2_666 ?
S11 O11 1.526(9) . ?
S11 C11 1.696(18) . ?
S11 C12 1.780(15) . ?
S21 O21 1.513(10) . ?
S21 C21 1.747(16) . ?
S21 C22 1.776(14) . ?
S31 O31 1.492(9) . ?
S31 C31 1.780(13) . ?
S31 C32 1.778(15) . ?
S41 O41 1.453(13) . ?
S41 C41 1.728(17) . ?
S41 C42 1.78(2) . ?
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.'
