#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:35:12 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179797 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/93/7009341.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_7009341
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            'C56 H40 Cu N4 P2 S4'
_chemical_formula_weight         1022.64
_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                 96.92(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.148(2)
_cell_length_b                   15.318(3)
_cell_length_c                   14.587(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.66
_cell_measurement_theta_min      1.98
_cell_volume                     2472.8(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       ω--2θ
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1437
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4347
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubes
_exptl_crystal_F_000             1054
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0117P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                2188
_reflns_number_total             4347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000093k.txt
_cod_data_source_block           2
_cod_original_cell_volume        2472.7(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7009341
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.0000 0.0000 0.05738(19) Uani 1 2 d S . .
S1 S 0.10391(8) -0.00051(7) -0.12587(6) 0.0703(3) Uani 1 1 d . . .
S2 S 0.13398(9) 0.09877(7) 0.06818(7) 0.0757(3) Uani 1 1 d . . .
P1 P 0.50305(7) 0.05611(6) -0.29106(6) 0.0451(2) Uani 1 1 d . . .
N1 N 0.0772(3) -0.0950(3) -0.3613(2) 0.0941(12) Uani 1 1 d . . .
N2 N 0.1959(3) 0.2216(2) 0.2870(2) 0.0856(11) Uani 1 1 d . . .
C1 C 0.0175(3) -0.0715(2) -0.1979(2) 0.0564(9) Uani 1 1 d . . .
C2 C 0.0512(3) -0.0853(3) -0.2887(3) 0.0661(11) Uani 1 1 d . . .
C3 C 0.0819(3) 0.1127(2) 0.1740(2) 0.0538(9) Uani 1 1 d . . .
C4 C 0.1465(3) 0.1728(3) 0.2372(3) 0.0623(10) Uani 1 1 d . . .
C5 C 0.4970(3) 0.0945(2) -0.1751(2) 0.0471(8) Uani 1 1 d . . .
C6 C 0.4064(3) 0.1497(3) -0.1560(2) 0.0712(11) Uani 1 1 d . . .
H6A H 0.3504 0.1700 -0.2036 0.085 Uiso 1 1 calc R . .
C7 C 0.3985(4) 0.1752(3) -0.0654(3) 0.0857(13) Uani 1 1 d . . .
H7A H 0.3369 0.2124 -0.0523 0.103 Uiso 1 1 calc R . .
C8 C 0.4801(4) 0.1460(3) 0.0032(3) 0.0748(12) Uani 1 1 d . . .
H8A H 0.4741 0.1631 0.0636 0.090 Uiso 1 1 calc R . .
C9 C 0.5709(4) 0.0920(3) -0.0145(3) 0.0725(11) Uani 1 1 d . . .
H9A H 0.6282 0.0739 0.0333 0.087 Uiso 1 1 calc R . .
C10 C 0.5783(3) 0.0642(2) -0.1033(2) 0.0609(10) Uani 1 1 d . . .
H10A H 0.6382 0.0249 -0.1149 0.073 Uiso 1 1 calc R . .
C11 C 0.4765(3) -0.0591(2) -0.2925(2) 0.0437(8) Uani 1 1 d . . .
C12 C 0.5404(3) -0.1158(2) -0.3421(2) 0.0626(10) Uani 1 1 d . . .
H12A H 0.6032 -0.0950 -0.3727 0.075 Uiso 1 1 calc R . .
C13 C 0.5111(3) -0.2027(3) -0.3463(3) 0.0764(11) Uani 1 1 d . . .
H13A H 0.5541 -0.2407 -0.3799 0.092 Uiso 1 1 calc R . .
C14 C 0.4191(3) -0.2340(3) -0.3016(3) 0.0739(11) Uani 1 1 d . . .
H14A H 0.3992 -0.2929 -0.3055 0.089 Uiso 1 1 calc R . .
C15 C 0.3561(3) -0.1791(3) -0.2510(3) 0.0683(11) Uani 1 1 d . . .
H15A H 0.2942 -0.2009 -0.2202 0.082 Uiso 1 1 calc R . .
C16 C 0.3843(3) -0.0918(3) -0.2457(2) 0.0595(9) Uani 1 1 d . . .
H16A H 0.3419 -0.0545 -0.2109 0.071 Uiso 1 1 calc R . .
C17 C 0.3858(3) 0.1085(2) -0.3668(2) 0.0470(8) Uani 1 1 d . . .
C18 C 0.2853(3) 0.0631(3) -0.4043(2) 0.0646(10) Uani 1 1 d . . .
H18A H 0.2756 0.0049 -0.3885 0.078 Uiso 1 1 calc R . .
C19 C 0.1991(3) 0.1037(3) -0.4652(3) 0.0805(12) Uani 1 1 d . . .
H19A H 0.1321 0.0724 -0.4914 0.097 Uiso 1 1 calc R . .
C20 C 0.2108(4) 0.1893(3) -0.4875(3) 0.0786(13) Uani 1 1 d . . .
H20A H 0.1519 0.2163 -0.5286 0.094 Uiso 1 1 calc R . .
C21 C 0.3100(4) 0.2360(3) -0.4493(3) 0.0787(12) Uani 1 1 d . . .
H21A H 0.3181 0.2946 -0.4639 0.094 Uiso 1 1 calc R . .
C22 C 0.3969(3) 0.1953(3) -0.3893(2) 0.0662(10) Uani 1 1 d . . .
H22A H 0.4641 0.2266 -0.3636 0.079 Uiso 1 1 calc R . .
C23 C 0.6444(3) 0.08068(19) -0.3325(2) 0.0464(8) Uani 1 1 d . . .
C24 C 0.6447(3) 0.1025(3) -0.4238(2) 0.0673(10) Uani 1 1 d . . .
H24A H 0.5724 0.1033 -0.4629 0.081 Uiso 1 1 calc R . .
C25 C 0.7516(4) 0.1232(3) -0.4584(3) 0.0862(13) Uani 1 1 d . . .
H25A H 0.7507 0.1381 -0.5203 0.103 Uiso 1 1 calc R . .
C26 C 0.8567(4) 0.1218(3) -0.4023(3) 0.0776(12) Uani 1 1 d . . .
H26A H 0.9282 0.1364 -0.4256 0.093 Uiso 1 1 calc R . .
C27 C 0.8595(3) 0.0994(3) -0.3121(3) 0.0764(12) Uani 1 1 d . . .
H27A H 0.9328 0.0975 -0.2742 0.092 Uiso 1 1 calc R . .
C28 C 0.7533(3) 0.0793(2) -0.2765(3) 0.0716(12) Uani 1 1 d . . .
H28A H 0.7553 0.0647 -0.2144 0.086 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'
Cu Cu 0.3201 1.2651 '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 Cu1 S2 180.0 . 3 ?
S2 Cu1 S1 90.92(4) . 3 ?
S2 Cu1 S1 89.08(4) 3 3 ?
S2 Cu1 S1 89.07(4) . . ?
S2 Cu1 S1 90.92(4) 3 . ?
S1 Cu1 S1 180.000(1) 3 . ?
C1 S1 Cu1 101.06(11) . . ?
C3 S2 Cu1 101.53(13) . . ?
C11 P1 C23 110.71(14) . . ?
C11 P1 C17 109.06(15) . . ?
C23 P1 C17 107.62(15) . . ?
C11 P1 C5 107.96(15) . . ?
C23 P1 C5 112.44(15) . . ?
C17 P1 C5 109.00(15) . . ?
C3 C1 C2 118.8(3) 3 . ?
C3 C1 S1 123.4(3) 3 . ?
C2 C1 S1 117.8(3) . . ?
N1 C2 C1 178.9(5) . . ?
C1 C3 C4 119.7(3) 3 . ?
C1 C3 S2 123.1(3) 3 . ?
C4 C3 S2 117.2(3) . . ?
N2 C4 C3 178.6(4) . . ?
C6 C5 C10 119.0(3) . . ?
C6 C5 P1 120.2(3) . . ?
C10 C5 P1 120.6(3) . . ?
C5 C6 C7 119.9(4) . . ?
C8 C7 C6 119.9(4) . . ?
C7 C8 C9 121.0(4) . . ?
C8 C9 C10 119.9(4) . . ?
C9 C10 C5 120.2(4) . . ?
C12 C11 C16 119.2(3) . . ?
C12 C11 P1 122.1(2) . . ?
C16 C11 P1 118.6(3) . . ?
C13 C12 C11 119.9(3) . . ?
C14 C13 C12 120.5(4) . . ?
C15 C14 C13 120.4(4) . . ?
C14 C15 C16 120.0(3) . . ?
C15 C16 C11 119.9(3) . . ?
C18 C17 C22 119.1(3) . . ?
C18 C17 P1 121.1(3) . . ?
C22 C17 P1 119.8(3) . . ?
C17 C18 C19 120.0(4) . . ?
C20 C19 C18 120.7(4) . . ?
C19 C20 C21 119.9(4) . . ?
C22 C21 C20 119.5(4) . . ?
C21 C22 C17 120.9(4) . . ?
C24 C23 C28 118.2(3) . . ?
C24 C23 P1 118.9(3) . . ?
C28 C23 P1 122.9(3) . . ?
C23 C24 C25 120.8(4) . . ?
C26 C25 C24 119.9(4) . . ?
C25 C26 C27 120.6(4) . . ?
C26 C27 C28 120.0(4) . . ?
C23 C28 C27 120.4(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
Cu1 S2 2.2695(11) . ?
Cu1 S2 2.2695(11) 3 ?
Cu1 S1 2.2860(10) 3 ?
Cu1 S1 2.2860(10) . ?
S1 C1 1.724(4) . ?
S2 C3 1.726(3) . ?
P1 C11 1.789(3) . ?
P1 C23 1.794(3) . ?
P1 C17 1.796(3) . ?
P1 C5 1.800(3) . ?
N1 C2 1.141(4) . ?
N2 C4 1.137(4) . ?
C1 C3 1.357(4) 3 ?
C1 C2 1.435(5) . ?
C3 C1 1.357(4) 3 ?
C3 C4 1.434(5) . ?
C5 C6 1.371(4) . ?
C5 C10 1.380(4) . ?
C6 C7 1.391(5) . ?
C7 C8 1.345(5) . ?
C8 C9 1.356(5) . ?
C9 C10 1.374(4) . ?
C11 C12 1.382(4) . ?
C11 C16 1.394(4) . ?
C12 C13 1.370(5) . ?
C13 C14 1.367(5) . ?
C14 C15 1.366(5) . ?
C15 C16 1.374(5) . ?
C17 C18 1.375(4) . ?
C17 C22 1.378(4) . ?
C18 C19 1.376(5) . ?
C19 C20 1.361(5) . ?
C20 C21 1.377(5) . ?
C21 C22 1.374(5) . ?
C23 C24 1.374(4) . ?
C23 C28 1.379(4) . ?
C24 C25 1.385(5) . ?
C25 C26 1.346(5) . ?
C26 C27 1.357(5) . ?
C27 C28 1.384(5) . ?
