#------------------------------------------------------------------------------
#$Date: 2025-08-22 14:50:14 +0200 (Fri, 22 Aug 2025) $
#$Revision: 301863 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/20/48/7204823.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_7204823
loop_
_publ_author_name
'Holmes, Kathryn E.'
'Kelly, Paul F.'
'Elsegood, Mark R. J.'
_publ_section_title
;
 Concomitant polymorphism of [Cu(Ph2SNH)4][PF6]2
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              56
_journal_paper_doi               10.1039/b316215j
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C48 H44 Cu F12 N4 P2 S4'
_chemical_formula_weight         1158.59
_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 except NH coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'All non-H atoms found by direct methods'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.398(2)
_cell_angle_beta                 103.569(2)
_cell_angle_gamma                92.897(2)
_cell_formula_units_Z            1
_cell_length_a                   8.8849(7)
_cell_length_b                   10.8557(9)
_cell_length_c                   13.3120(11)
_cell_measurement_reflns_used    6157
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.92
_cell_measurement_theta_min      2.36
_cell_volume                     1245.66(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11067
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             591
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0317
_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)+(0.0363P)²+0.6590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                4705
_reflns_number_total             5765
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b316215j.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204823
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
Cu1 Cu 0.5000 0.5000 0.5000 0.02230(8) Uani 1 2 d S . .
N1 N 0.3896(2) 0.33139(14) 0.48655(12) 0.0251(3) Uani 1 1 d . . .
H1A H 0.295(3) 0.336(2) 0.4846(18) 0.038 Uiso 1 1 d . . .
S1 S 0.45367(5) 0.21302(4) 0.54917(3) 0.02358(10) Uani 1 1 d . . .
C1 C 0.4186(2) 0.21761(16) 0.67676(13) 0.0227(4) Uani 1 1 d . . .
C2 C 0.2782(2) 0.2541(2) 0.69072(15) 0.0329(4) Uani 1 1 d . . .
H2 H 0.1978 0.2729 0.6332 0.040 Uiso 1 1 calc R . .
C3 C 0.2568(3) 0.2628(2) 0.79060(17) 0.0414(5) Uani 1 1 d . . .
H3 H 0.1611 0.2878 0.8020 0.050 Uiso 1 1 calc R . .
C4 C 0.3747(3) 0.2352(2) 0.87345(15) 0.0368(5) Uani 1 1 d . . .
H4 H 0.3585 0.2399 0.9414 0.044 Uiso 1 1 calc R . .
C5 C 0.5149(2) 0.20101(18) 0.85888(15) 0.0324(4) Uani 1 1 d . . .
H5 H 0.5955 0.1836 0.9166 0.039 Uiso 1 1 calc R . .
C6 C 0.5388(2) 0.19182(17) 0.75944(15) 0.0280(4) Uani 1 1 d . . .
H6 H 0.6354 0.1684 0.7484 0.034 Uiso 1 1 calc R . .
C7 C 0.3196(2) 0.08589(17) 0.49312(14) 0.0263(4) Uani 1 1 d . . .
C8 C 0.2956(2) -0.01458(18) 0.55132(16) 0.0323(4) Uani 1 1 d . . .
H8 H 0.3461 -0.0159 0.6226 0.039 Uiso 1 1 calc R . .
C9 C 0.1971(3) -0.11268(19) 0.50388(17) 0.0375(5) Uani 1 1 d . . .
H9 H 0.1791 -0.1815 0.5431 0.045 Uiso 1 1 calc R . .
C10 C 0.1246(3) -0.1117(2) 0.40031(17) 0.0395(5) Uani 1 1 d . . .
H10 H 0.0579 -0.1800 0.3685 0.047 Uiso 1 1 calc R . .
C11 C 0.1485(3) -0.0118(2) 0.34278(17) 0.0461(6) Uani 1 1 d . . .
H11 H 0.0978 -0.0111 0.2715 0.055 Uiso 1 1 calc R . .
C12 C 0.2465(3) 0.0876(2) 0.38896(16) 0.0402(5) Uani 1 1 d . . .
H12 H 0.2635 0.1565 0.3495 0.048 Uiso 1 1 calc R . .
N2 N 0.4452(2) 0.50956(15) 0.35023(12) 0.0299(4) Uani 1 1 d . . .
H2A H 0.503(3) 0.551(2) 0.3229(19) 0.045 Uiso 1 1 d . . .
S2 S 0.34499(5) 0.40643(4) 0.27085(3) 0.02388(10) Uani 1 1 d . . .
C13 C 0.4715(2) 0.30384(16) 0.22861(13) 0.0245(4) Uani 1 1 d . . .
C14 C 0.6308(2) 0.3230(2) 0.26338(15) 0.0330(4) Uani 1 1 d . . .
H14 H 0.6745 0.3924 0.3073 0.040 Uiso 1 1 calc R . .
C15 C 0.7256(3) 0.2385(2) 0.23260(17) 0.0440(6) Uani 1 1 d . . .
H15 H 0.8351 0.2502 0.2557 0.053 Uiso 1 1 calc R . .
C16 C 0.6614(3) 0.1379(2) 0.16866(18) 0.0448(6) Uani 1 1 d . . .
H16 H 0.7269 0.0810 0.1477 0.054 Uiso 1 1 calc R . .
C17 C 0.5018(3) 0.11957(19) 0.13498(17) 0.0398(5) Uani 1 1 d . . .
H17 H 0.4584 0.0504 0.0907 0.048 Uiso 1 1 calc R . .
C18 C 0.4055(2) 0.20163(17) 0.16567(14) 0.0294(4) Uani 1 1 d . . .
H18 H 0.2960 0.1883 0.1441 0.035 Uiso 1 1 calc R . .
C19 C 0.2710(2) 0.48834(16) 0.15574(13) 0.0235(4) Uani 1 1 d . . .
C20 C 0.3249(2) 0.47813(18) 0.06661(14) 0.0278(4) Uani 1 1 d . . .
H20 H 0.4037 0.4236 0.0624 0.033 Uiso 1 1 calc R . .
C21 C 0.2614(2) 0.54936(19) -0.01700(15) 0.0312(4) Uani 1 1 d . . .
H21 H 0.2962 0.5427 -0.0790 0.037 Uiso 1 1 calc R . .
C22 C 0.1482(2) 0.62945(18) -0.01006(16) 0.0324(4) Uani 1 1 d . . .
H22 H 0.1061 0.6781 -0.0672 0.039 Uiso 1 1 calc R . .
C23 C 0.0956(2) 0.63931(19) 0.07960(17) 0.0336(4) Uani 1 1 d . . .
H23 H 0.0185 0.6953 0.0842 0.040 Uiso 1 1 calc R . .
C24 C 0.1553(2) 0.56740(18) 0.16280(15) 0.0306(4) Uani 1 1 d . . .
H24 H 0.1175 0.5721 0.2238 0.037 Uiso 1 1 calc R . .
P1 P 0.0000 0.5000 0.5000 0.03063(16) Uani 1 2 d S . .
F1 F 0.04640(18) 0.46975(14) 0.61936(11) 0.0548(4) Uani 1 1 d . . .
F2 F 0.17586(14) 0.54379(12) 0.50538(12) 0.0495(4) Uani 1 1 d . . .
F3 F 0.03457(14) 0.36182(11) 0.46955(11) 0.0422(3) Uani 1 1 d . . .
P2 P 0.0000 0.0000 0.0000 0.02833(15) Uani 1 2 d S . .
F4 F 0.15766(16) -0.05196(13) 0.06259(12) 0.0547(4) Uani 1 1 d . . .
F5 F 0.01507(16) 0.10839(13) 0.08613(11) 0.0488(3) Uani 1 1 d . . .
F6 F 0.09426(19) 0.08619(14) -0.06131(13) 0.0644(5) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 '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
N2 Cu1 N2 180.000(1) . 2_666 ?
N2 Cu1 N1 89.46(6) . . ?
N2 Cu1 N1 90.54(6) 2_666 . ?
N2 Cu1 N1 90.54(6) . 2_666 ?
N2 Cu1 N1 89.46(6) 2_666 2_666 ?
N1 Cu1 N1 180.0 . 2_666 ?
S1 N1 Cu1 125.54(10) . . ?
N1 S1 C1 111.11(8) . . ?
N1 S1 C7 105.50(9) . . ?
C1 S1 C7 98.97(8) . . ?
C2 C1 C6 121.91(17) . . ?
C2 C1 S1 119.69(14) . . ?
C6 C1 S1 118.26(14) . . ?
C1 C2 C3 118.56(18) . . ?
C4 C3 C2 120.1(2) . . ?
C5 C4 C3 120.93(19) . . ?
C4 C5 C6 119.94(18) . . ?
C1 C6 C5 118.59(18) . . ?
C12 C7 C8 120.56(18) . . ?
C12 C7 S1 118.45(15) . . ?
C8 C7 S1 120.91(15) . . ?
C9 C8 C7 118.95(19) . . ?
C10 C9 C8 120.7(2) . . ?
C9 C10 C11 120.2(2) . . ?
C10 C11 C12 120.0(2) . . ?
C11 C12 C7 119.6(2) . . ?
S2 N2 Cu1 125.60(9) . . ?
N2 S2 C13 109.78(9) . . ?
N2 S2 C19 104.30(8) . . ?
C13 S2 C19 101.97(8) . . ?
C14 C13 C18 121.41(18) . . ?
C14 C13 S2 120.14(15) . . ?
C18 C13 S2 118.34(15) . . ?
C13 C14 C15 118.6(2) . . ?
C16 C15 C14 120.4(2) . . ?
C15 C16 C17 120.3(2) . . ?
C18 C17 C16 120.2(2) . . ?
C17 C18 C13 119.0(2) . . ?
C20 C19 C24 121.22(17) . . ?
C20 C19 S2 124.01(15) . . ?
C24 C19 S2 114.75(14) . . ?
C19 C20 C21 118.80(18) . . ?
C22 C21 C20 120.34(18) . . ?
C21 C22 C23 120.38(18) . . ?
C22 C23 C24 120.06(19) . . ?
C23 C24 C19 119.18(18) . . ?
F1 P1 F1 180.000(1) . 2_566 ?
F1 P1 F2 89.76(8) . . ?
F1 P1 F2 90.24(8) 2_566 . ?
F1 P1 F2 90.24(8) . 2_566 ?
F1 P1 F2 89.76(8) 2_566 2_566 ?
F2 P1 F2 180.0 . 2_566 ?
F1 P1 F3 90.20(7) . . ?
F1 P1 F3 89.80(7) 2_566 . ?
F2 P1 F3 90.01(7) . . ?
F2 P1 F3 89.99(7) 2_566 . ?
F1 P1 F3 89.80(7) . 2_566 ?
F1 P1 F3 90.20(7) 2_566 2_566 ?
F2 P1 F3 89.99(7) . 2_566 ?
F2 P1 F3 90.01(7) 2_566 2_566 ?
F3 P1 F3 180.00(10) . 2_566 ?
F6 P2 F6 180.00(13) 2 . ?
F6 P2 F4 89.94(9) 2 . ?
F6 P2 F4 90.06(9) . . ?
F6 P2 F4 90.06(9) 2 2 ?
F6 P2 F4 89.94(9) . 2 ?
F4 P2 F4 180.00(15) . 2 ?
F6 P2 F5 89.57(8) 2 2 ?
F6 P2 F5 90.43(8) . 2 ?
F4 P2 F5 89.74(7) . 2 ?
F4 P2 F5 90.26(7) 2 2 ?
F6 P2 F5 90.43(8) 2 . ?
F6 P2 F5 89.57(8) . . ?
F4 P2 F5 90.26(7) . . ?
F4 P2 F5 89.74(7) 2 . ?
F5 P2 F5 180.00(12) 2 . ?
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 N2 1.9449(15) . ?
Cu1 N2 1.9449(15) 2_666 ?
Cu1 N1 2.0162(16) . ?
Cu1 N1 2.0162(16) 2_666 ?
N1 S1 1.6043(16) . ?
S1 C1 1.7973(18) . ?
S1 C7 1.8020(19) . ?
C1 C2 1.380(3) . ?
C1 C6 1.387(3) . ?
C2 C3 1.388(3) . ?
C3 C4 1.382(3) . ?
C4 C5 1.372(3) . ?
C5 C6 1.391(3) . ?
C7 C12 1.387(3) . ?
C7 C8 1.389(3) . ?
C8 C9 1.383(3) . ?
C9 C10 1.379(3) . ?
C10 C11 1.379(3) . ?
C11 C12 1.386(3) . ?
N2 S2 1.6008(16) . ?
S2 C13 1.7923(19) . ?
S2 C19 1.7956(18) . ?
C13 C14 1.386(3) . ?
C13 C18 1.391(3) . ?
C14 C15 1.393(3) . ?
C15 C16 1.381(4) . ?
C16 C17 1.385(4) . ?
C17 C18 1.384(3) . ?
C19 C20 1.384(3) . ?
C19 C24 1.390(3) . ?
C20 C21 1.395(3) . ?
C21 C22 1.380(3) . ?
C22 C23 1.384(3) . ?
C23 C24 1.388(3) . ?
P1 F1 1.5919(13) . ?
P1 F1 1.5919(13) 2_566 ?
P1 F2 1.5948(13) . ?
P1 F2 1.5948(13) 2_566 ?
P1 F3 1.6075(12) . ?
P1 F3 1.6075(12) 2_566 ?
P2 F6 1.5880(13) 2 ?
P2 F6 1.5880(13) . ?
P2 F4 1.5905(13) . ?
P2 F4 1.5905(13) 2 ?
P2 F5 1.6010(13) 2 ?
P2 F5 1.6010(13) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A F3 0.84(2) 2.31(2) 3.144(2) 175(2) .
N1 H1A F2 0.84(2) 2.57(2) 3.102(2) 122(2) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139195528
