#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:35:12 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179797 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/93/7009348.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_7009348
loop_
_publ_author_name
'Lewis, Gareth R.'
'Dance, Ian'
_publ_section_title
;
 Crystal supramolecular motifs for [Ph4P]+ salts of [M(mnt)2]2−,
 [M(mnt)2]−, [{M(mnt)2}2]2−, [M(mnt)3]3− and
 [M(mnt)3]2−
 (mnt2− = maleonitriledithiolate) †
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3176
_journal_paper_doi               10.1039/b000093k
_journal_year                    2000
_chemical_formula_sum            'C60 H40 Cr N6 P2 S6'
_chemical_formula_weight         1151.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.290(5)
_cell_length_b                   15.548(4)
_cell_length_c                   17.986(4)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.02
_cell_volume                     5674(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT+'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.1510
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38090
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.421591
_exptl_absorpt_correction_type   SADBAS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubes
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         3720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.840
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0644P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1859
_reflns_number_gt                1863
_reflns_number_total             3720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000093k.txt
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7009348
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
Cr1 Cr 1.0000 1.66490(8) -0.2500 0.0818(5) Uani 1 2 d S . .
S1 S 1.05414(8) 1.68193(10) -0.36360(11) 0.0884(6) Uani 1 1 d . . .
S2 S 0.94315(9) 1.55570(11) -0.31089(11) 0.0967(6) Uani 1 1 d . . .
S3 S 0.92418(8) 1.76682(10) -0.29774(11) 0.0863(6) Uani 1 1 d . . .
N1 N 1.1732(3) 1.8199(4) -0.4634(4) 0.115(2) Uani 1 1 d . . .
N2 N 0.7939(4) 1.9180(4) -0.2371(4) 0.136(3) Uani 1 1 d . . .
N3 N 0.9365(4) 1.3215(5) -0.3362(6) 0.182(4) Uani 1 1 d . . .
P1 P 0.86508(8) 1.83203(9) -0.59810(10) 0.0737(5) Uani 1 1 d . . .
C1 C 1.1090(3) 1.7656(3) -0.3488(4) 0.0735(17) Uani 1 1 d . . .
C2 C 1.1447(3) 1.7952(4) -0.4130(5) 0.088(2) Uani 1 1 d . . .
C3 C 0.8806(3) 1.7987(4) -0.2184(4) 0.0761(18) Uani 1 1 d . . .
C4 C 0.8318(4) 1.8663(4) -0.2307(4) 0.095(2) Uani 1 1 d . . .
C5 C 0.9780(3) 1.4628(4) -0.2773(4) 0.089(2) Uani 1 1 d . . .
C6 C 0.9546(4) 1.3837(5) -0.3106(6) 0.132(3) Uani 1 1 d . . .
C13 C 0.8786(3) 1.7199(4) -0.5851(4) 0.0809(18) Uani 1 1 d . . .
C14 C 0.9146(4) 1.6906(4) -0.5230(5) 0.115(3) Uani 1 1 d . . .
H14A H 0.9315 1.7297 -0.4888 0.138 Uiso 1 1 calc R . .
C15 C 0.9245(4) 1.6028(5) -0.5131(5) 0.123(3) Uani 1 1 d . . .
H15A H 0.9480 1.5830 -0.4721 0.148 Uiso 1 1 calc R . .
C16 C 0.9003(5) 1.5466(5) -0.5627(6) 0.121(3) Uani 1 1 d . . .
H16A H 0.9079 1.4881 -0.5562 0.145 Uiso 1 1 calc R . .
C17 C 0.8644(4) 1.5741(4) -0.6228(5) 0.111(3) Uani 1 1 d . . .
H17A H 0.8471 1.5345 -0.6563 0.133 Uiso 1 1 calc R . .
C18 C 0.8543(3) 1.6607(4) -0.6330(4) 0.090(2) Uani 1 1 d . . .
H18A H 0.8300 1.6791 -0.6738 0.108 Uiso 1 1 calc R . .
C19 C 0.8170(3) 1.8732(4) -0.5231(4) 0.0748(17) Uani 1 1 d . . .
C20 C 0.7854(4) 1.8217(5) -0.4728(5) 0.115(3) Uani 1 1 d . . .
H20A H 0.7923 1.7625 -0.4737 0.138 Uiso 1 1 calc R . .
C21 C 0.7434(5) 1.8573(5) -0.4209(5) 0.141(3) Uani 1 1 d . . .
H21A H 0.7207 1.8214 -0.3884 0.169 Uiso 1 1 calc R . .
C22 C 0.7347(4) 1.9426(5) -0.4164(5) 0.118(3) Uani 1 1 d . . .
H22A H 0.7083 1.9659 -0.3792 0.141 Uiso 1 1 calc R . .
C23 C 0.7643(4) 1.9940(4) -0.4663(4) 0.098(2) Uani 1 1 d . . .
H23A H 0.7563 2.0529 -0.4651 0.118 Uiso 1 1 calc R . .
C24 C 0.8063(3) 1.9611(4) -0.5192(4) 0.094(2) Uani 1 1 d . . .
H24A H 0.8275 1.9978 -0.5523 0.113 Uiso 1 1 calc R . .
C25 C 0.9390(3) 1.8936(4) -0.6058(4) 0.0724(17) Uani 1 1 d . . .
C26 C 0.9385(3) 1.9687(5) -0.6444(5) 0.112(3) Uani 1 1 d . . .
H26A H 0.9006 1.9849 -0.6699 0.134 Uiso 1 1 calc R . .
C27 C 0.9932(4) 2.0213(5) -0.6466(5) 0.117(3) Uani 1 1 d . . .
H27A H 0.9915 2.0730 -0.6725 0.140 Uiso 1 1 calc R . .
C28 C 1.0490(4) 1.9983(5) -0.6117(5) 0.103(2) Uani 1 1 d . . .
H28A H 1.0860 2.0336 -0.6135 0.124 Uiso 1 1 calc R . .
C29 C 1.0507(4) 1.9245(6) -0.5745(5) 0.124(3) Uani 1 1 d . . .
H29A H 1.0893 1.9087 -0.5502 0.148 Uiso 1 1 calc R . .
C30 C 0.9973(4) 1.8712(5) -0.5710(5) 0.111(3) Uani 1 1 d . . .
H30A H 1.0001 1.8195 -0.5452 0.134 Uiso 1 1 calc R . .
C31 C 0.8183(3) 1.8451(3) -0.6816(4) 0.0675(17) Uani 1 1 d . . .
C32 C 0.7529(3) 1.8641(4) -0.6783(4) 0.0810(19) Uani 1 1 d . . .
H32A H 0.7328 1.8729 -0.6324 0.097 Uiso 1 1 calc R . .
C33 C 0.7160(4) 1.8705(4) -0.7426(6) 0.091(2) Uani 1 1 d . . .
H33A H 0.6714 1.8841 -0.7403 0.109 Uiso 1 1 calc R . .
C34 C 0.7464(5) 1.8566(4) -0.8110(5) 0.097(2) Uani 1 1 d . . .
H34A H 0.7220 1.8603 -0.8546 0.117 Uiso 1 1 calc R . .
C35 C 0.8112(5) 1.8376(5) -0.8141(4) 0.101(2) Uani 1 1 d . . .
H35A H 0.8308 1.8277 -0.8600 0.121 Uiso 1 1 calc R . .
C36 C 0.8489(3) 1.8327(4) -0.7501(5) 0.090(2) Uani 1 1 d . . .
H36A H 0.8938 1.8213 -0.7528 0.108 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'
P P 0.1023 0.0942 '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'
Cr Cr 0.3209 0.6236 '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
S2 Cr1 S2 86.26(11) . 3_754 ?
S2 Cr1 S1 84.50(6) . . ?
S2 Cr1 S1 105.15(7) 3_754 . ?
S2 Cr1 S1 105.15(7) . 3_754 ?
S2 Cr1 S1 84.50(7) 3_754 3_754 ?
S1 Cr1 S1 166.98(10) . 3_754 ?
S2 Cr1 S3 89.75(7) . . ?
S2 Cr1 S3 168.66(6) 3_754 . ?
S1 Cr1 S3 84.98(7) . . ?
S1 Cr1 S3 86.32(7) 3_754 . ?
S2 Cr1 S3 168.67(6) . 3_754 ?
S2 Cr1 S3 89.75(7) 3_754 3_754 ?
S1 Cr1 S3 86.32(7) . 3_754 ?
S1 Cr1 S3 84.98(7) 3_754 3_754 ?
S3 Cr1 S3 96.06(9) . 3_754 ?
C1 S1 Cr1 104.6(3) . . ?
C5 S2 Cr1 104.1(2) . . ?
C3 S3 Cr1 102.8(2) . . ?
C13 P1 C25 113.9(3) . . ?
C13 P1 C19 109.7(3) . . ?
C25 P1 C19 109.0(3) . . ?
C13 P1 C31 107.7(3) . . ?
C25 P1 C31 108.7(3) . . ?
C19 P1 C31 107.7(3) . . ?
C3 C1 C2 121.7(6) 3_754 . ?
C3 C1 S1 122.2(6) 3_754 . ?
C2 C1 S1 116.1(5) . . ?
N1 C2 C1 178.9(8) . . ?
C1 C3 C4 121.6(6) 3_754 . ?
C1 C3 S3 123.4(5) 3_754 . ?
C4 C3 S3 115.0(6) . . ?
N2 C4 C3 177.2(9) . . ?
C5 C5 C6 121.8(5) 3_754 . ?
C5 C5 S2 122.5(2) 3_754 . ?
C6 C5 S2 115.7(6) . . ?
N3 C6 C5 179.4(13) . . ?
C18 C13 C14 118.3(6) . . ?
C18 C13 P1 121.7(6) . . ?
C14 C13 P1 120.0(5) . . ?
C15 C14 C13 119.5(7) . . ?
C16 C15 C14 120.1(8) . . ?
C15 C16 C17 121.0(7) . . ?
C18 C17 C16 119.4(8) . . ?
C13 C18 C17 121.7(7) . . ?
C20 C19 C24 118.2(6) . . ?
C20 C19 P1 123.1(5) . . ?
C24 C19 P1 118.5(5) . . ?
C19 C20 C21 120.1(7) . . ?
C22 C21 C20 121.3(8) . . ?
C21 C22 C23 119.3(7) . . ?
C22 C23 C24 121.1(7) . . ?
C23 C24 C19 119.9(6) . . ?
C26 C25 C30 117.1(6) . . ?
C26 C25 P1 119.6(5) . . ?
C30 C25 P1 123.3(5) . . ?
C25 C26 C27 121.2(7) . . ?
C28 C27 C26 120.5(7) . . ?
C29 C28 C27 119.1(7) . . ?
C28 C29 C30 121.8(7) . . ?
C29 C30 C25 120.3(7) . . ?
C32 C31 C36 120.2(6) . . ?
C32 C31 P1 120.4(6) . . ?
C36 C31 P1 119.4(5) . . ?
C31 C32 C33 120.5(7) . . ?
C32 C33 C34 119.2(7) . . ?
C35 C34 C33 120.2(7) . . ?
C34 C35 C36 121.1(8) . . ?
C35 C36 C31 118.7(7) . . ?
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
Cr1 S2 2.327(2) . ?
Cr1 S2 2.327(2) 3_754 ?
Cr1 S1 2.3348(19) . ?
Cr1 S1 2.3349(19) 3_754 ?
Cr1 S3 2.3695(19) . ?
Cr1 S3 2.3696(19) 3_754 ?
S1 C1 1.732(6) . ?
S2 C5 1.718(6) . ?
S3 C3 1.750(7) . ?
N1 C2 1.141(8) . ?
N2 C4 1.118(8) . ?
N3 C6 1.133(9) . ?
P1 C13 1.781(6) . ?
P1 C25 1.785(6) . ?
P1 C19 1.784(7) . ?
P1 C31 1.789(6) . ?
C1 C3 1.331(8) 3_754 ?
C1 C2 1.440(10) . ?
C3 C1 1.331(8) 3_754 ?
C3 C4 1.461(10) . ?
C5 C5 1.328(13) 3_754 ?
C5 C6 1.447(10) . ?
C13 C18 1.354(8) . ?
C13 C14 1.409(9) . ?
C14 C15 1.391(9) . ?
C15 C16 1.342(11) . ?
C16 C17 1.371(10) . ?
C17 C18 1.375(8) . ?
C19 C20 1.367(9) . ?
C19 C24 1.385(8) . ?
C20 C21 1.381(10) . ?
C21 C22 1.340(9) . ?
C22 C23 1.344(9) . ?
C23 C24 1.376(9) . ?
C25 C26 1.358(8) . ?
C25 C30 1.382(8) . ?
C26 C27 1.380(8) . ?
C27 C28 1.342(9) . ?
C28 C29 1.329(9) . ?
C29 C30 1.366(9) . ?
C31 C32 1.362(8) . ?
C31 C36 1.393(9) . ?
C32 C33 1.381(9) . ?
C33 C34 1.393(9) . ?
C34 C35 1.347(10) . ?
C35 C36 1.384(9) . ?
