#------------------------------------------------------------------------------
#$Date: 2019-11-24 09:59:11 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237551 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/84/4088411.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_4088411
loop_
_publ_author_name
'Chambers, Geoffrey M.'
'Rauchfuss, Thomas B.'
'Arrigoni, Federica'
'Zampella, Giuseppe'
_publ_section_title
;
 Effect of Pyramidalization of the M2(SR)2Center: The Case of
 (C5H5)2Ni2(SR)2
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              836
_journal_paper_doi               10.1021/acs.organomet.6b00068
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C16 H22 Ni3 S4'
_chemical_formula_sum            'C16 H22 Ni3 S4'
_chemical_formula_weight         518.71
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.321(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.6021(16)
_cell_length_b                   19.865(6)
_cell_length_c                   8.345(2)
_cell_measurement_reflns_used    5352
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.65
_cell_volume                     928.7(4)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  bm85tas
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10140
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    3.454
_exptl_absorpt_correction_T_max  0.8760
_exptl_absorpt_correction_T_min  0.5700
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             532
_exptl_crystal_id                bm85tas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-2 1 0 ) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0177
_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)+(0.0242P)²+0.3879P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0446
_refine_ls_wR_factor_ref         0.0460
_reflns_number_gt                1559
_reflns_number_total             1688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           bm85tas
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        928.6(5)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               4088411
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
Ni1 Ni -0.02077(4) -0.120025(12) 0.18134(3) 0.02051(9) Uani 1 1 d .
Ni2 Ni 0.0000 0.0000 0.0000 0.01692(10) Uani 1 2 d S
S1 S -0.26720(8) -0.08017(2) 0.00132(6) 0.02144(12) Uani 1 1 d .
S2 S -0.00551(8) -0.01498(2) 0.26044(6) 0.02056(12) Uani 1 1 d .
C1 C -0.0971(4) -0.22130(11) 0.2677(3) 0.0374(6) Uani 1 1 d .
H1 H -0.2588 -0.2406 0.2885 0.045 Uiso 1 1 calc R
C2 C 0.0474(4) -0.18880(12) 0.3781(3) 0.0396(6) Uani 1 1 d .
H2 H 0.0098 -0.1807 0.4935 0.047 Uiso 1 1 calc R
C3 C 0.2638(4) -0.16881(11) 0.2962(3) 0.0335(5) Uani 1 1 d .
H3 H 0.4045 -0.1462 0.3470 0.040 Uiso 1 1 calc R
C4 C 0.2524(3) -0.19237(10) 0.1395(3) 0.0286(5) Uani 1 1 d .
H4 H 0.3813 -0.1894 0.0574 0.034 Uiso 1 1 calc R
C5 C 0.0231(4) -0.22059(10) 0.1179(3) 0.0313(5) Uani 1 1 d .
H5 H -0.0373 -0.2417 0.0168 0.038 Uiso 1 1 calc R
C6 C -0.2257(4) -0.12194(10) -0.1926(2) 0.0273(5) Uani 1 1 d .
H6A H -0.0530 -0.1266 -0.2144 0.033 Uiso 1 1 calc R
H6B H -0.2963 -0.1676 -0.1888 0.033 Uiso 1 1 calc R
C7 C -0.3447(4) -0.08116(10) -0.3279(2) 0.0293(5) Uani 1 1 d .
H7A H -0.2861 -0.0984 -0.4318 0.035 Uiso 1 1 calc R
H7B H -0.5190 -0.0892 -0.3245 0.035 Uiso 1 1 calc R
C8 C -0.3009(3) -0.00529(10) -0.3214(2) 0.0245(4) Uani 1 1 d .
H8A H -0.4135 0.0154 -0.2447 0.029 Uiso 1 1 calc R
H8B H -0.3329 0.0143 -0.4285 0.029 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'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 0.00 0.1300
-1.00 0.00 0.00 0.1170
0.00 1.00 0.00 0.0170
0.00 -1.00 0.00 0.0210
0.00 0.00 -1.00 0.0710
0.00 0.00 1.00 0.0490
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
C5 Ni1 C3 65.26(8) . .
C5 Ni1 C4 39.17(8) . .
C3 Ni1 C4 38.41(8) . .
C5 Ni1 C2 64.36(9) . .
C3 Ni1 C2 39.74(9) . .
C4 Ni1 C2 64.85(8) . .
C5 Ni1 C1 38.92(9) . .
C3 Ni1 C1 64.64(9) . .
C4 Ni1 C1 64.77(8) . .
C2 Ni1 C1 37.09(9) . .
C5 Ni1 S1 104.37(6) . .
C3 Ni1 S1 163.73(7) . .
C4 Ni1 S1 125.75(6) . .
C2 Ni1 S1 149.05(7) . .
C1 Ni1 S1 115.95(7) . .
C5 Ni1 S2 170.61(6) . .
C3 Ni1 S2 105.95(6) . .
C4 Ni1 S2 131.72(6) . .
C2 Ni1 S2 111.46(7) . .
C1 Ni1 S2 141.91(7) . .
S1 Ni1 S2 83.41(2) . .
C5 Ni1 Ni2 131.93(6) . .
C3 Ni1 Ni2 127.02(6) . .
C4 Ni1 Ni2 116.73(6) . .
C2 Ni1 Ni2 158.33(7) . .
C1 Ni1 Ni2 164.59(7) . .
S1 Ni1 Ni2 49.723(15) . .
S2 Ni1 Ni2 49.91(2) . .
S1 Ni2 S1 180.0 3 .
S1 Ni2 S2 83.267(18) 3 3
S1 Ni2 S2 96.733(18) . 3
S1 Ni2 S2 96.735(18) 3 .
S1 Ni2 S2 83.265(18) . .
S2 Ni2 S2 180.0 3 .
S1 Ni2 Ni1 130.357(17) 3 .
S1 Ni2 Ni1 49.643(17) . .
S2 Ni2 Ni1 130.205(15) 3 .
S2 Ni2 Ni1 49.793(15) . .
S1 Ni2 Ni1 49.643(17) 3 3
S1 Ni2 Ni1 130.357(17) . 3
S2 Ni2 Ni1 49.795(15) 3 3
S2 Ni2 Ni1 130.207(15) . 3
Ni1 Ni2 Ni1 180.0 . 3
C6 S1 Ni1 111.11(7) . .
C6 S1 Ni2 103.60(7) . .
Ni1 S1 Ni2 80.63(2) . .
C8 S2 Ni1 109.14(6) 3 .
C8 S2 Ni2 103.12(7) 3 .
Ni1 S2 Ni2 80.30(2) . .
C2 C1 C5 107.61(19) . .
C2 C1 Ni1 70.98(13) . .
C5 C1 Ni1 66.79(11) . .
C2 C1 H1 126.2 . .
C5 C1 H1 126.2 . .
Ni1 C1 H1 126.2 . .
C1 C2 C3 107.6(2) . .
C1 C2 Ni1 71.93(13) . .
C3 C2 Ni1 67.36(11) . .
C1 C2 H2 126.2 . .
C3 C2 H2 126.2 . .
Ni1 C2 H2 126.2 . .
C4 C3 C2 108.47(19) . .
C4 C3 Ni1 72.20(12) . .
C2 C3 Ni1 72.90(12) . .
C4 C3 H3 125.6 . .
C2 C3 H3 125.6 . .
Ni1 C3 H3 125.6 . .
C3 C4 C5 106.91(19) . .
C3 C4 Ni1 69.39(11) . .
C5 C4 Ni1 68.58(11) . .
C3 C4 H4 126.5 . .
C5 C4 H4 126.5 . .
Ni1 C4 H4 126.5 . .
C4 C5 C1 109.0(2) . .
C4 C5 Ni1 72.25(12) . .
C1 C5 Ni1 74.29(13) . .
C4 C5 H5 125.3 . .
C1 C5 H5 125.3 . .
Ni1 C5 H5 125.3 . .
C7 C6 S1 110.64(14) . .
C7 C6 H6A 109.5 . .
S1 C6 H6A 109.5 . .
C7 C6 H6B 109.5 . .
S1 C6 H6B 109.5 . .
H6A C6 H6B 108.1 . .
C8 C7 C6 115.14(16) . .
C8 C7 H7A 108.5 . .
C6 C7 H7A 108.5 . .
C8 C7 H7B 108.5 . .
C6 C7 H7B 108.5 . .
H7A C7 H7B 107.5 . .
C7 C8 S2 112.12(13) . 3
C7 C8 H8A 109.2 . .
S2 C8 H8A 109.2 3 .
C7 C8 H8B 109.2 . .
S2 C8 H8B 109.2 3 .
H8A C8 H8B 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 C5 2.081(2) .
Ni1 C3 2.093(2) .
Ni1 C4 2.1294(19) .
Ni1 C2 2.168(2) .
Ni1 C1 2.180(2) .
Ni1 S1 2.1831(6) .
Ni1 S2 2.1901(8) .
Ni1 Ni2 2.8267(7) .
Ni2 S1 2.1857(6) 3
Ni2 S1 2.1857(6) .
Ni2 S2 2.1939(8) 3
Ni2 S2 2.1939(8) .
Ni2 Ni1 2.8268(7) 3
S1 C6 1.834(2) .
S2 C8 1.832(2) 3
C1 C2 1.383(4) .
C1 C5 1.423(3) .
C1 H1 1.0000 .
C2 C3 1.450(3) .
C2 H2 1.0000 .
C3 C4 1.390(3) .
C3 H3 1.0000 .
C4 C5 1.412(3) .
C4 H4 1.0000 .
C5 H5 1.0000 .
C6 C7 1.538(3) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.528(3) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 S2 1.8324(19) 3
C8 H8A 0.9900 .
C8 H8B 0.9900 .
