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#$Date: 2016-03-26 01:57:47 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180116 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/14/7101420.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_7101420
loop_
_publ_author_name
'Wolfram Willy Seidel'
'Tania Pape'
'Markus Schaffrath'
_publ_section_title
;
Acetylenedithiolate alkyne complex formation
renders it a dithiolate chelate ligand
;
_journal_issue                   38
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b606068d
_journal_year                    2006
_chemical_formula_sum            'C52 H60 B2 N12 Ni O4 S4 W2'
_chemical_formula_weight         1493.39
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.751(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1411(17)
_cell_length_b                   18.928(3)
_cell_length_c                   15.605(3)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     2932.6(9)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33188
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    4.427
_exptl_absorpt_correction_T_max  0.7771
_exptl_absorpt_correction_T_min  0.5564
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.644
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         8547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0480
_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)+(0.0391P)²+7.1498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                7142
_reflns_number_total             8547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b606068d.txt
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7101420
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 0.5000 0.5000 0.5000 0.01912(17) Uani 1 2 d S
S1 S 0.65364(12) 0.54833(6) 0.60451(8) 0.0242(2) Uani 1 1 d .
S2 S 0.54598(13) 0.39185(6) 0.55164(8) 0.0254(3) Uani 1 1 d .
C1 C 0.7175(4) 0.4768(2) 0.6624(3) 0.0202(9) Uani 1 1 d .
C2 C 0.6726(5) 0.4103(2) 0.6363(3) 0.0213(9) Uani 1 1 d .
W1 W 0.827945(18) 0.404932(9) 0.742379(11) 0.01825(6) Uani 1 1 d .
C3 C 0.7919(5) 0.3089(3) 0.6883(3) 0.0271(10) Uani 1 1 d .
C4 C 0.6825(5) 0.3862(3) 0.8104(3) 0.0256(10) Uani 1 1 d .
O3 O 0.7674(4) 0.2549(2) 0.6553(3) 0.0415(10) Uani 1 1 d .
O4 O 0.5981(4) 0.3744(2) 0.8467(3) 0.0404(10) Uani 1 1 d .
B1 B 1.1420(5) 0.4461(3) 0.8309(4) 0.0242(11) Uani 1 1 d .
H1 H 1.2373 0.4585 0.8579 0.029 Uiso 1 1 calc R
N1 N 1.0020(4) 0.4227(2) 0.6816(3) 0.0232(8) Uani 1 1 d .
N2 N 1.1227(4) 0.4447(2) 0.7307(3) 0.0245(8) Uani 1 1 d .
C5 C 0.9080(6) 0.3958(3) 0.5250(3) 0.0372(13) Uani 1 1 d .
H5A H 0.8838 0.3469 0.5355 0.056 Uiso 1 1 calc R
H5B H 0.9391 0.3986 0.4696 0.056 Uiso 1 1 calc R
H5C H 0.8290 0.4263 0.5220 0.056 Uiso 1 1 calc R
C6 C 1.0178(5) 0.4198(3) 0.5979(3) 0.0271(10) Uani 1 1 d .
C7 C 1.1465(6) 0.4408(3) 0.5937(4) 0.0340(12) Uani 1 1 d .
H7 H 1.1833 0.4443 0.5426 0.041 Uiso 1 1 calc R
C8 C 1.2112(5) 0.4557(3) 0.6783(3) 0.0280(11) Uani 1 1 d .
C9 C 1.3536(5) 0.4782(3) 0.7126(4) 0.0405(14) Uani 1 1 d .
H9A H 1.3553 0.5158 0.7560 0.061 Uiso 1 1 calc R
H9B H 1.3928 0.4957 0.6642 0.061 Uiso 1 1 calc R
H9C H 1.4061 0.4378 0.7401 0.061 Uiso 1 1 calc R
N3 N 0.9759(4) 0.3487(2) 0.8434(3) 0.0237(8) Uani 1 1 d .
N4 N 1.1072(4) 0.3722(2) 0.8618(3) 0.0239(8) Uani 1 1 d .
C10 C 0.8510(5) 0.2436(3) 0.8843(4) 0.0348(12) Uani 1 1 d .
H10A H 0.7751 0.2754 0.8856 0.052 Uiso 1 1 calc R
H10B H 0.8658 0.2130 0.9360 0.052 Uiso 1 1 calc R
H10C H 0.8309 0.2146 0.8312 0.052 Uiso 1 1 calc R
C11 C 0.9741(5) 0.2860(3) 0.8842(3) 0.0253(10) Uani 1 1 d .
C12 C 1.1040(5) 0.2700(3) 0.9284(3) 0.0275(10) Uani 1 1 d .
H12 H 1.1314 0.2293 0.9631 0.033 Uiso 1 1 calc R
C13 C 1.1848(5) 0.3243(3) 0.9122(3) 0.0246(10) Uani 1 1 d .
C14 C 1.3345(5) 0.3318(3) 0.9402(4) 0.0363(13) Uani 1 1 d .
H14A H 1.3761 0.3271 0.8891 0.054 Uiso 1 1 calc R
H14B H 1.3692 0.2948 0.9828 0.054 Uiso 1 1 calc R
H14C H 1.3560 0.3783 0.9670 0.054 Uiso 1 1 calc R
N5 N 0.9094(4) 0.4937(2) 0.8286(2) 0.0215(8) Uani 1 1 d .
N6 N 1.0462(4) 0.5001(2) 0.8576(2) 0.0233(8) Uani 1 1 d .
C15 C 0.7031(5) 0.5592(3) 0.8478(4) 0.0329(12) Uani 1 1 d .
H15A H 0.6689 0.5649 0.7848 0.049 Uiso 1 1 calc R
H15B H 0.6847 0.6022 0.8784 0.049 Uiso 1 1 calc R
H15C H 0.6583 0.5189 0.8692 0.049 Uiso 1 1 calc R
C16 C 0.8513(5) 0.5464(3) 0.8647(3) 0.0256(10) Uani 1 1 d .
C17 C 0.9509(6) 0.5870(3) 0.9165(3) 0.0319(12) Uani 1 1 d .
H17 H 0.9376 0.6276 0.9494 0.038 Uiso 1 1 calc R
C18 C 1.0720(6) 0.5571(3) 0.9109(3) 0.0285(11) Uani 1 1 d .
C19 C 1.2114(6) 0.5805(3) 0.9516(4) 0.0399(14) Uani 1 1 d .
H19A H 1.2588 0.5420 0.9871 0.060 Uiso 1 1 calc R
H19B H 1.2069 0.6217 0.9889 0.060 Uiso 1 1 calc R
H19C H 1.2600 0.5930 0.9055 0.060 Uiso 1 1 calc R
C21 C -0.0258(7) 0.6447(4) 0.6964(4) 0.0567(19) Uani 1 1 d .
H21A H -0.0576 0.6658 0.6385 0.085 Uiso 1 1 calc R
H21B H -0.0950 0.6502 0.7315 0.085 Uiso 1 1 calc R
H21C H -0.0077 0.5943 0.6898 0.085 Uiso 1 1 calc R
C22 C 0.1011(7) 0.6809(4) 0.7413(4) 0.0447(15) Uani 1 1 d .
C23 C 0.2236(7) 0.6620(4) 0.7243(4) 0.0460(15) Uani 1 1 d .
H23 H 0.2286 0.6254 0.6834 0.055 Uiso 1 1 calc R
C24 C 0.3418(8) 0.6962(5) 0.7664(5) 0.063(2) Uani 1 1 d .
H24 H 0.4264 0.6831 0.7540 0.075 Uiso 1 1 calc R
C25 C 0.3342(10) 0.7483(5) 0.8253(6) 0.078(3) Uani 1 1 d .
H25 H 0.4135 0.7719 0.8541 0.094 Uiso 1 1 calc R
C26 C 0.2111(11) 0.7667(4) 0.8432(6) 0.078(3) Uani 1 1 d .
H26 H 0.2060 0.8026 0.8848 0.094 Uiso 1 1 calc R
C27 C 0.0971(8) 0.7336(4) 0.8014(5) 0.0586(19) Uani 1 1 d .
H27 H 0.0129 0.7472 0.8140 0.070 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
W W -0.8490 6.8722 '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
S1 Ni1 S1 180.0 3_666 .
S1 Ni1 S2 87.16(4) 3_666 .
S1 Ni1 S2 92.84(4) . .
S1 Ni1 S2 92.84(4) 3_666 3_666
S1 Ni1 S2 87.16(4) . 3_666
S2 Ni1 S2 180.00(6) . 3_666
C1 S1 Ni1 101.51(16) . .
C2 S2 Ni1 99.49(16) . .
C2 C1 S1 120.7(3) . .
C2 C1 W1 71.0(3) . .
S1 C1 W1 167.6(3) . .
C1 C2 S2 125.3(4) . .
C1 C2 W1 69.5(3) . .
S2 C2 W1 165.2(3) . .
C3 W1 C4 88.4(2) . .
C3 W1 C1 108.62(18) . .
C4 W1 C1 94.07(19) . .
C3 W1 C2 70.08(18) . .
C4 W1 C2 84.81(19) . .
C1 W1 C2 39.47(18) . .
C3 W1 N1 92.92(18) . .
C4 W1 N1 173.73(17) . .
C1 W1 N1 91.32(16) . .
C2 W1 N1 101.42(17) . .
C3 W1 N5 163.85(17) . .
C4 W1 N5 92.05(17) . .
C1 W1 N5 87.46(17) . .
C2 W1 N5 126.04(16) . .
N1 W1 N5 84.96(15) . .
C3 W1 N3 84.42(17) . .
C4 W1 N3 90.17(17) . .
C1 W1 N3 166.37(17) . .
C2 W1 N3 154.10(16) . .
N1 W1 N3 83.86(15) . .
N5 W1 N3 79.44(14) . .
O3 C3 W1 177.5(4) . .
O4 C4 W1 177.8(5) . .
N6 B1 N2 109.5(4) . .
N6 B1 N4 108.9(4) . .
N2 B1 N4 108.1(4) . .
C6 N1 N2 106.6(4) . .
C6 N1 W1 132.6(3) . .
N2 N1 W1 120.7(3) . .
C8 N2 N1 109.7(4) . .
C8 N2 B1 130.7(4) . .
N1 N2 B1 119.3(4) . .
N1 C6 C7 109.5(5) . .
N1 C6 C5 122.3(5) . .
C7 C6 C5 128.2(5) . .
C6 C7 C8 106.5(5) . .
N2 C8 C7 107.7(5) . .
N2 C8 C9 122.7(5) . .
C7 C8 C9 129.6(5) . .
C11 N3 N4 106.9(4) . .
C11 N3 W1 133.4(3) . .
N4 N3 W1 118.6(3) . .
C13 N4 N3 109.3(4) . .
C13 N4 B1 130.5(4) . .
N3 N4 B1 120.0(4) . .
N3 C11 C12 108.9(4) . .
N3 C11 C10 124.6(4) . .
C12 C11 C10 126.4(4) . .
C13 C12 C11 106.6(4) . .
N4 C13 C12 108.2(4) . .
N4 C13 C14 123.0(4) . .
C12 C13 C14 128.7(4) . .
C16 N5 N6 107.2(4) . .
C16 N5 W1 133.0(3) . .
N6 N5 W1 119.7(3) . .
C18 N6 N5 109.2(4) . .
C18 N6 B1 130.3(4) . .
N5 N6 B1 120.5(4) . .
N5 C16 C17 109.0(5) . .
N5 C16 C15 124.0(4) . .
C17 C16 C15 126.9(5) . .
C18 C17 C16 106.9(5) . .
N6 C18 C17 107.7(4) . .
N6 C18 C19 123.0(5) . .
C17 C18 C19 129.3(5) . .
C23 C22 C27 118.4(7) . .
C23 C22 C21 121.0(7) . .
C27 C22 C21 120.6(7) . .
C22 C23 C24 120.7(7) . .
C25 C24 C23 119.4(8) . .
C24 C25 C26 119.9(8) . .
C27 C26 C25 120.3(9) . .
C26 C27 C22 121.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S1 2.2112(12) 3_666
Ni1 S1 2.2112(12) .
Ni1 S2 2.2145(12) .
Ni1 S2 2.2145(12) 3_666
S1 C1 1.682(5) .
S2 C2 1.680(5) .
C1 C2 1.373(6) .
C1 W1 2.024(5) .
C2 W1 2.043(4) .
W1 C3 2.006(5) .
W1 C4 2.016(5) .
W1 N1 2.193(4) .
W1 N5 2.205(4) .
W1 N3 2.216(4) .
C3 O3 1.148(6) .
C4 O4 1.140(6) .
B1 N6 1.525(7) .
B1 N2 1.536(7) .
B1 N4 1.545(7) .
N1 C6 1.350(6) .
N1 N2 1.370(6) .
N2 C8 1.348(6) .
C5 C6 1.491(8) .
C6 C7 1.378(7) .
C7 C8 1.379(8) .
C8 C9 1.497(8) .
N3 C11 1.348(6) .
N3 N4 1.377(5) .
N4 C13 1.344(6) .
C10 C11 1.484(7) .
C11 C12 1.390(7) .
C12 C13 1.370(7) .
C13 C14 1.498(7) .
N5 C16 1.340(6) .
N5 N6 1.374(5) .
N6 C18 1.355(6) .
C15 C16 1.492(7) .
C16 C17 1.388(7) .
C17 C18 1.371(8) .
C18 C19 1.494(8) .
C21 C22 1.501(10) .
C22 C23 1.371(9) .
C22 C27 1.375(10) .
C23 C24 1.402(10) .
C24 C25 1.361(12) .
C25 C26 1.377(13) .
C26 C27 1.358(12) .
