#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100744.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_1100744
loop_
_publ_author_name
'Stéphane A. Baudron'
'Narcis Avarvari'
'Patrick Batail'
_publ_contact_author
; Dr Patrick Batail 

  Laboratoire Chimie Ingénierie Moléculaires et

  Matériaux d'Angers,

  UMR 6200 CNRS-Université d'Angers,

  Bat. K, 2, Boulevard Lavoisier, Angers, France 

;
_publ_contact_author_email       patrick.batail@univ-angers.fr
_publ_contact_author_fax         '33 2 41 73 50 11'
_publ_contact_author_phone       '33 2 41 73 52 64'
_publ_section_title
;

A Straightforward Synthesis of Diverse Nickel Dithiolene Complexes Appended

with Hydrogen-Bond Donor/Acceptor Groups

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3380
_journal_page_last               3382
_journal_paper_doi               10.1021/ic050174n
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H76 N6 Ni O2 S4'
_chemical_formula_weight         860.02
_chemical_name_common            (n-Bu4N)[Ni(mant)2]
_chemical_name_systematic
;

 ?

;
_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                70.09(3)
_cell_angle_beta                 77.79(2)
_cell_angle_gamma                76.68(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1252(17)
_cell_length_b                   11.804(3)
_cell_length_c                   12.478(3)
_cell_measurement_reflns_used    3495
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      2.1
_cell_volume                     1216.7(5)
_computing_cell_refinement       'SELECT, CELL [STOE-IPDS]'
_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, Phi. incr. = 1.9'
_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  0.1174
_diffrn_reflns_av_sigmaI/netI    0.2538
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12471
_diffrn_reflns_theta_full        26.23
_diffrn_reflns_theta_max         26.23
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_correction_T_min  0.9061
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, STOE-IPDS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       platelet
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.2694
_exptl_crystal_size_mid          0.1156
_exptl_crystal_size_min          0.0230
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.592
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.592
_refine_ls_R_factor_all          0.1528
_refine_ls_R_factor_gt           0.0414
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                1579
_reflns_number_total             4462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050174nsi20050201_114543.cif
_cod_data_source_block           sb687e
_cod_original_cell_volume        1216.6(4)
_cod_database_code               1100744
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 0.0000 0.0000 0.0000 0.0402(3) Uani 1 2 d S . .
S1 S 0.05150(13) -0.09573(10) 0.17306(11) 0.0479(4) Uani 1 1 d . . .
S2 S 0.16269(14) -0.13469(10) -0.06560(11) 0.0476(4) Uani 1 1 d . . .
C1 C 0.2218(5) -0.3105(4) 0.2675(5) 0.0499(14) Uani 1 1 d . . .
C2 C 0.1793(5) -0.2270(4) 0.1604(4) 0.0423(13) Uani 1 1 d . . .
C3 C 0.2308(5) -0.2429(4) 0.0535(4) 0.0408(12) Uani 1 1 d . . .
C4 C 0.3448(5) -0.3529(4) 0.0397(4) 0.0408(12) Uani 1 1 d . . .
O1 O 0.4011(3) -0.4343(3) 0.1195(3) 0.0548(10) Uani 1 1 d . . .
N1 N 0.2470(5) -0.3697(4) 0.3581(4) 0.0698(14) Uani 1 1 d . . .
N2 N 0.3883(5) -0.3558(3) -0.0701(4) 0.0638(13) Uani 1 1 d . . .
H2A H 0.4559 -0.4149 -0.0846 0.077 Uiso 1 1 calc R . .
H2B H 0.3485 -0.2986 -0.1254 0.077 Uiso 1 1 calc R . .
N1B N 0.7164(4) -0.3439(3) 0.2453(3) 0.0369(9) Uani 1 1 d . . .
C1B C 0.8283(5) -0.3383(4) 0.1345(3) 0.0427(12) Uani 1 1 d . . .
H1B1 H 0.8673 -0.2622 0.1096 0.051 Uiso 1 1 calc R . .
H1B2 H 0.9136 -0.4047 0.1515 0.051 Uiso 1 1 calc R . .
C2B C 0.7628(5) -0.3466(4) 0.0350(4) 0.0513(13) Uani 1 1 d . . .
H2B1 H 0.6716 -0.2855 0.0215 0.062 Uiso 1 1 calc R . .
H2B2 H 0.7351 -0.4266 0.0549 0.062 Uiso 1 1 calc R . .
C3B C 0.8796(5) -0.3258(4) -0.0745(4) 0.0583(14) Uani 1 1 d . . .
H3B1 H 0.9039 -0.2445 -0.0956 0.070 Uiso 1 1 calc R . .
H3B2 H 0.9724 -0.3844 -0.0593 0.070 Uiso 1 1 calc R . .
C4B C 0.8215(5) -0.3388(5) -0.1742(4) 0.0656(15) Uani 1 1 d . . .
H4B1 H 0.8976 -0.3244 -0.2412 0.098 Uiso 1 1 calc R . .
H4B2 H 0.7303 -0.2802 -0.1901 0.098 Uiso 1 1 calc R . .
H4B3 H 0.8000 -0.4199 -0.1545 0.098 Uiso 1 1 calc R . .
C5B C 0.6524(5) -0.4624(4) 0.2900(3) 0.0431(11) Uani 1 1 d . . .
H5B1 H 0.5834 -0.4624 0.3608 0.052 Uiso 1 1 calc R . .
H5B2 H 0.5926 -0.4624 0.2343 0.052 Uiso 1 1 calc R . .
C6B C 0.7670(5) -0.5809(4) 0.3138(4) 0.0529(13) Uani 1 1 d . . .
H6B1 H 0.8272 -0.5890 0.2419 0.063 Uiso 1 1 calc R . .
H6B2 H 0.8353 -0.5793 0.3629 0.063 Uiso 1 1 calc R . .
C7B C 0.6849(6) -0.6895(4) 0.3723(4) 0.0668(15) Uani 1 1 d . . .
H7B1 H 0.6084 -0.6845 0.3268 0.080 Uiso 1 1 calc R . .
H7B2 H 0.6327 -0.6841 0.4471 0.080 Uiso 1 1 calc R . .
C8B C 0.7889(7) -0.8133(5) 0.3887(5) 0.101(2) Uani 1 1 d . . .
H8B1 H 0.7297 -0.8772 0.4263 0.151 Uiso 1 1 calc R . .
H8B2 H 0.8639 -0.8200 0.4351 0.151 Uiso 1 1 calc R . .
H8B3 H 0.8387 -0.8208 0.3149 0.151 Uiso 1 1 calc R . .
C9B C 0.8043(5) -0.3328(4) 0.3307(3) 0.0434(12) Uani 1 1 d . . .
H9B1 H 0.8408 -0.2554 0.2989 0.052 Uiso 1 1 calc R . .
H9B2 H 0.8927 -0.3974 0.3389 0.052 Uiso 1 1 calc R . .
C10B C 0.7154(6) -0.3397(4) 0.4499(4) 0.0599(14) Uani 1 1 d . . .
H10A H 0.6918 -0.4214 0.4877 0.072 Uiso 1 1 calc R . .
H10B H 0.6201 -0.2826 0.4424 0.072 Uiso 1 1 calc R . .
C11B C 0.8060(7) -0.3096(5) 0.5239(4) 0.0725(16) Uani 1 1 d . . .
H11A H 0.7635 -0.3400 0.6044 0.087 Uiso 1 1 calc R . .
H11B H 0.9105 -0.3512 0.5145 0.087 Uiso 1 1 calc R . .
C12B C 0.8043(8) -0.1741(5) 0.4926(5) 0.106(2) Uani 1 1 d . . .
H12A H 0.8636 -0.1598 0.5402 0.159 Uiso 1 1 calc R . .
H12B H 0.7013 -0.1327 0.5045 0.159 Uiso 1 1 calc R . .
H12C H 0.8468 -0.1436 0.4132 0.159 Uiso 1 1 calc R . .
C13B C 0.5808(5) -0.2416(4) 0.2237(4) 0.0457(12) Uani 1 1 d . . .
H13A H 0.5136 -0.2476 0.2962 0.055 Uiso 1 1 calc R . .
H13B H 0.5256 -0.2553 0.1720 0.055 Uiso 1 1 calc R . .
C14B C 0.6136(5) -0.1117(4) 0.1731(4) 0.0580(14) Uani 1 1 d . . .
H14A H 0.6744 -0.0977 0.2210 0.070 Uiso 1 1 calc R . .
H14B H 0.6719 -0.1013 0.0968 0.070 Uiso 1 1 calc R . .
C15B C 0.4672(5) -0.0185(4) 0.1654(4) 0.0639(16) Uani 1 1 d . . .
H15A H 0.4011 -0.0397 0.1263 0.077 Uiso 1 1 calc R . .
H15B H 0.4911 0.0614 0.1193 0.077 Uiso 1 1 calc R . .
C16B C 0.3822(7) -0.0111(5) 0.2822(5) 0.104(2) Uani 1 1 d . . .
H16A H 0.2909 0.0488 0.2717 0.156 Uiso 1 1 calc R . .
H16B H 0.4457 0.0120 0.3207 0.156 Uiso 1 1 calc R . .
H16C H 0.3561 -0.0894 0.3279 0.156 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'
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'
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
S1 Ni1 S1 180.00(6) . 2 ?
S1 Ni1 S2 88.90(5) . 2 ?
S1 Ni1 S2 91.10(5) 2 2 ?
S1 Ni1 S2 91.10(5) . . ?
S1 Ni1 S2 88.90(5) 2 . ?
S2 Ni1 S2 180.00(9) 2 . ?
C2 S1 Ni1 104.18(17) . . ?
C3 S2 Ni1 105.32(15) . . ?
N1 C1 C2 173.5(5) . . ?
C3 C2 C1 125.7(4) . . ?
C3 C2 S1 120.0(3) . . ?
C1 C2 S1 114.3(3) . . ?
C2 C3 C4 121.1(4) . . ?
C2 C3 S2 119.2(3) . . ?
C4 C3 S2 119.7(3) . . ?
O1 C4 N2 120.5(4) . . ?
O1 C4 C3 124.4(4) . . ?
N2 C4 C3 115.0(4) . . ?
C13B N1B C9B 111.3(3) . . ?
C13B N1B C5B 106.0(3) . . ?
C9B N1B C5B 111.7(3) . . ?
C13B N1B C1B 110.7(3) . . ?
C9B N1B C1B 106.1(3) . . ?
C5B N1B C1B 111.1(3) . . ?
C2B C1B N1B 115.2(4) . . ?
C1B C2B C3B 110.4(4) . . ?
C4B C3B C2B 112.1(4) . . ?
C6B C5B N1B 116.8(3) . . ?
C7B C6B C5B 110.2(4) . . ?
C6B C7B C8B 114.1(4) . . ?
N1B C9B C10B 115.4(4) . . ?
C9B C10B C11B 111.3(4) . . ?
C12B C11B C10B 112.5(4) . . ?
N1B C13B C14B 117.0(4) . . ?
C15B C14B C13B 111.2(4) . . ?
C14B C15B C16B 113.4(4) . . ?
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 S1 2.1640(14) . ?
Ni1 S1 2.1640(14) 2 ?
Ni1 S2 2.1648(12) 2 ?
Ni1 S2 2.1648(12) . ?
S1 C2 1.744(4) . ?
S2 C3 1.720(5) . ?
C1 N1 1.148(5) . ?
C1 C2 1.433(6) . ?
C2 C3 1.379(6) . ?
C3 C4 1.500(5) . ?
C4 O1 1.231(4) . ?
C4 N2 1.353(5) . ?
N1B C13B 1.514(4) . ?
N1B C9B 1.518(5) . ?
N1B C5B 1.522(5) . ?
N1B C1B 1.527(5) . ?
C1B C2B 1.526(5) . ?
C2B C3B 1.529(6) . ?
C3B C4B 1.516(6) . ?
C5B C6B 1.521(5) . ?
C6B C7B 1.520(6) . ?
C7B C8B 1.522(6) . ?
C9B C10B 1.521(6) . ?
C10B C11B 1.532(6) . ?
C11B C12B 1.508(6) . ?
C13B C14B 1.521(6) . ?
C14B C15B 1.520(6) . ?
C15B C16B 1.520(6) . ?
