#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/00/2240029.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2240029
loop_
_publ_author_name
'Corfield, Peter W. R.'
_publ_section_title
;
 Crystal structure of
 poly[(μ₃-thiocyanato-κ³N:S:S)(trimethylphosphine
 sulfide-κS)copper(I)]
;
_journal_coeditor_code           PK2530
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              281
_journal_page_last               285
_journal_paper_doi               10.1107/S1600536814021412
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Cu (N C S) (C3 H9 P S)]'
_chemical_formula_moiety         'C4 H9 Cu1 N1 P1 S2'
_chemical_formula_sum            'C4 H9 Cu N P S2'
_chemical_formula_weight         229.75
_chemical_name_common
'trimethylposphinesulfidecopper(I) thiocyanate'
_chemical_name_systematic
;
Poly[(μ₃-thiocyanato-κ³N:S:S)(trimethylphosphine
sulfide-κS)copper(I)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.945(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   5.793(3)
_cell_length_b                   14.091(3)
_cell_length_c                   22.064(7)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      41.0
_cell_measurement_theta_min      6.4
_cell_volume                     1779.2(11)
_computing_cell_refinement
;
Corfield (1972)
;
_computing_data_collection
;
Corfield (1972)
;
_computing_data_reduction
;
Data reduction followed procedures in Corfield et al. (1973) with
 p =
0.06,
with programs written by Corfield and by Graeme Gainsford
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
local superposition program (Corfield, 1972)
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Picker 4-circle'
_diffrn_measurement_method       'θ/2θ scans'
_diffrn_radiation_monochromator  'oriented graphite 200 reflection'
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6315
_diffrn_reflns_theta_full        63.31
_diffrn_reflns_theta_max         63.31
_diffrn_reflns_theta_min         3.73
_diffrn_standards_decay_%        0.6(4)
_diffrn_standards_interval_count 400
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    8.73
_exptl_absorpt_correction_T_max  0.704
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(Busing & Levy, 1957)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_meas      1.709
_exptl_crystal_density_method    flotation
_exptl_crystal_description       rod
_exptl_crystal_F_000             928
_exptl_crystal_size_max          .31
_exptl_crystal_size_mid          .059
_exptl_crystal_size_min          .049
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.305
_refine_ls_extinction_coef       0.00128(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.787
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0265
_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)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                2144
_reflns_number_total             2912
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2530sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C4 H9 Cu1 N1 P1 S2'
_cod_database_code               2240029
_cod_database_fobs_code          2240029
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_group
Cu Cu1 0.03939(9) 0.30233(4) 0.41293(3) 0.04640(17) Uani d . 1 1 .
Cu Cu2A -0.2710(4) 0.3110(2) 0.25554(15) 0.0484(5) Uani d P 0.647(6) 1 1
Cu Cu2B -0.2599(8) 0.3379(3) 0.2721(2) 0.0484(5) Uani d P 0.353(6) 1 2
S S1 -0.17677(15) 0.43301(6) 0.37964(4) 0.0432(2) Uani d . 1 1 .
S S2 -0.11907(16) 0.39160(7) 0.18567(4) 0.0524(3) Uani d . 1 1 .
P P1 0.05098(15) 0.53894(6) 0.37911(4) 0.0356(2) Uani d . 1 1 .
P P2 -0.38568(14) 0.45343(6) 0.13294(4) 0.0326(2) Uani d . 1 1 .
S S3 -0.18043(14) 0.20640(6) 0.46933(4) 0.0440(2) Uani d . 1 1 .
S S4 0.01342(14) 0.21297(6) 0.30788(4) 0.0372(2) Uani d . 1 1 .
N N3 0.3696(5) 0.2829(2) 0.44265(13) 0.0448(7) Uani d . 1 1 .
C C3 0.5556(5) 0.2523(2) 0.45340(14) 0.0326(7) Uani d . 1 1 .
N N4 0.4265(5) 0.2852(2) 0.27391(14) 0.0488(8) Uani d . 1 1 .
C C4 0.2553(5) 0.2565(2) 0.28759(14) 0.0341(7) Uani d . 1 1 .
C C11 -0.1011(7) 0.6494(3) 0.3727(2) 0.0656(12) Uani d . 1 1 .
H H11A 0.0079 0.7001 0.3705 0.098 Uiso calc R 1 1 .
H H11B -0.1773 0.6582 0.4080 0.098 Uiso calc R 1 1 .
H H11C -0.2157 0.6492 0.3363 0.098 Uiso calc R 1 1 .
C C12 0.2638(7) 0.5438(3) 0.44721(16) 0.0566(11) Uani d . 1 1 .
H H12A 0.3472 0.4847 0.4523 0.085 Uiso calc R 1 1 .
H H12B 0.1868 0.5547 0.4821 0.085 Uiso calc R 1 1 .
H H12C 0.3716 0.5945 0.4438 0.085 Uiso calc R 1 1 .
C C13 0.2128(7) 0.5328(3) 0.31678(16) 0.0555(10) Uani d . 1 1 .
H H13A 0.1069 0.5336 0.2787 0.083 Uiso calc R 1 1 .
H H13B 0.3024 0.4752 0.3197 0.083 Uiso calc R 1 1 .
H H13C 0.3162 0.5863 0.3184 0.083 Uiso calc R 1 1 .
C C21 -0.5941(7) 0.3702(3) 0.09550(17) 0.0572(11) Uani d . 1 1 .
H H21A -0.7119 0.4035 0.0681 0.086 Uiso calc R 1 1 .
H H21B -0.6657 0.3369 0.1257 0.086 Uiso calc R 1 1 .
H H21C -0.5165 0.3257 0.0726 0.086 Uiso calc R 1 1 .
C C22 -0.2800(6) 0.5203(2) 0.07406(15) 0.0443(8) Uani d . 1 1 .
H H22A -0.4071 0.5546 0.0507 0.066 Uiso calc R 1 1 .
H H22B -0.2131 0.4780 0.0474 0.066 Uiso calc R 1 1 .
H H22C -0.1630 0.5643 0.0924 0.066 Uiso calc R 1 1 .
C C23 -0.5452(7) 0.5329(3) 0.17392(18) 0.0563(10) Uani d . 1 1 .
H H23A -0.4407 0.5795 0.1947 0.084 Uiso calc R 1 1 .
H H23B -0.6165 0.4979 0.2034 0.084 Uiso calc R 1 1 .
H H23C -0.6642 0.5639 0.1457 0.084 Uiso calc R 1 1 .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 1 -1
0 6 7
1 0 0
-1 1 1
0 6 -7
-1 0 0
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 Cu1 S1 . . 133.19(9) n
N3 Cu1 S3 . . 109.10(9) n
S1 Cu1 S3 . . 108.66(5) n
N3 Cu1 S4 . . 98.56(9) n
S1 Cu1 S4 . . 98.61(4) n
S3 Cu1 S4 . . 103.37(4) n
N4 Cu2A S2 1_455 . 137.01(15) n
N4 Cu2A S4 1_455 . 112.91(14) ?
S2 Cu2A S4 . . 108.98(10) ?
N4 Cu2B S2 1_455 . 125.7(3) ?
N4 Cu2B S4 1_455 . 106.2(2) ?
S2 Cu2B S4 . . 102.14(18) ?
N4 Cu2B S1 1_455 . 102.0(2) ?
S2 Cu2B S1 . . 121.57(19) ?
S4 Cu2B S1 . . 93.24(16) ?
P1 S1 Cu1 . . 105.99(5) y
P1 S1 Cu2B . . 113.21(11) ?
Cu1 S1 Cu2B . . 84.04(11) ?
P2 S2 Cu2A . . 106.09(8) y
P2 S2 Cu2B . . 106.55(13) y
C13 P1 C11 . . 107.1(2) ?
C13 P1 C12 . . 105.85(18) ?
C11 P1 C12 . . 107.5(2) ?
C13 P1 S1 . . 113.33(14) ?
C11 P1 S1 . . 109.55(15) ?
C12 P1 S1 . . 113.18(14) ?
C23 P2 C22 . . 107.47(18) ?
C23 P2 C21 . . 106.22(19) ?
C22 P2 C21 . . 107.02(17) ?
C23 P2 S2 . . 113.29(14) ?
C22 P2 S2 . . 109.52(12) ?
C21 P2 S2 . . 112.98(15) ?
C3 S3 Cu1 1_455 . 102.90(12) y
C4 S4 Cu2B . . 100.44(16) y
C4 S4 Cu2A . . 102.18(13) y
C4 S4 Cu1 . . 97.27(12) ?
Cu2B S4 Cu1 . . 83.30(12) ?
Cu2A S4 Cu1 . . 95.33(10) ?
C3 N3 Cu1 . . 164.6(3) y
N3 C3 S3 . 1_655 178.8(3) ?
C4 N4 Cu2A . 1_655 169.9(3) y
C4 N4 Cu2B . 1_655 166.1(3) y
Cu2A N4 Cu2B 1_655 1_655 15.43(11) ?
N4 C4 S4 . . 178.6(3) ?
P1 C11 H11A . . 109.5 ?
P1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
P1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
P1 C12 H12A . . 109.5 ?
P1 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
P1 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
P1 C13 H13A . . 109.5 ?
P1 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
P1 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
P2 C21 H21A . . 109.5 ?
P2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
P2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
P2 C22 H22A . . 109.5 ?
P2 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
P2 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
P2 C23 H23A . . 109.5 ?
P2 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
P2 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N3 . 1.943(3) y
Cu1 S1 . 2.2830(11) y
Cu1 S3 . 2.3431(11) y
Cu1 S4 . 2.6214(12) n
Cu1 Cu2B . 3.351(5) n
Cu1 Cu2A . 3.656(3) n
Cu2A N4 1_455 1.894(4) y
Cu2A S2 . 2.206(3) y
Cu2A S4 . 2.316(3) y
Cu2B N4 1_455 1.969(6) y
Cu2B S2 . 2.315(5) y
Cu2B S4 . 2.416(5) y
Cu2B S1 . 2.702(5) n
S1 P1 . 1.9935(13) y
S2 P2 . 1.9848(14) y
P1 C13 . 1.783(4) ?
P1 C11 . 1.783(4) ?
P1 C12 . 1.791(3) ?
P2 C23 . 1.784(4) ?
P2 C22 . 1.788(3) ?
P2 C21 . 1.790(3) ?
S3 C3 1_455 1.648(3) ?
S4 C4 . 1.654(3) ?
N3 C3 . 1.150(4) ?
N4 C4 . 1.154(4) ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
C21 H21A . 0.9600 ?
C21 H21B . 0.9600 ?
C21 H21C . 0.9600 ?
C22 H22A . 0.9600 ?
C22 H22B . 0.9600 ?
C22 H22C . 0.9600 ?
C23 H23A . 0.9600 ?
C23 H23B . 0.9600 ?
C23 H23C . 0.9600 ?
