#------------------------------------------------------------------------------
#$Date: 2017-01-09 06:53:52 +0200 (Mon, 09 Jan 2017) $
#$Revision: 190238 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/58/7055808.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_7055808
loop_
_publ_author_name
'Artem’ev, Alexander V.'
'Doronina, Evgeniya P.'
'Rakhmanova, Marianna I.'
'Sutyrina, Anastasiya O.'
'Bagryanskaya, Irina Yu.'
'Tolstoy, Peter M.'
'Gushchin, Artem L.'
'Mazur, Anton S.'
'Gusarova, Nina K.'
'Trofimov, Boris A.'
_publ_section_title
;
 Luminescent CuI thiocyanate complexes based on tris(2-pyridyl)phosphine
 and its oxide: from mono-, di- and trinuclear species to coordination
 polymers
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              10028
_journal_paper_doi               10.1039/C6NJ02087A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C32 H24 Cu2 N8 O2 P2 S2'
_chemical_formula_sum            'C32 H24 Cu2 N8 O2 P2 S2'
_chemical_formula_weight         805.73
_chemical_melting_point          482.15
_chemical_name_systematic
'copper(I) thiocyanate complex of  tris(2pyridyl)phosphine oxide'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2013
_audit_update_record
;
2015-07-14 deposited with the CCDC.
2016-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                71.147(3)
_cell_angle_beta                 78.454(3)
_cell_angle_gamma                65.128(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3784(8)
_cell_length_b                   9.0242(8)
_cell_length_c                   13.1937(11)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.58
_cell_volume                     854.08(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42492
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.583
_exptl_absorpt_coefficient_mu    1.504
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       prism
_exptl_crystal_F_000             408
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/hexane'
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.043
_refine_diff_density_max         2.450
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0921
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0894P)²+19.6032P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3304
_refine_ls_wR_factor_ref         0.3340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3230
_reflns_number_total             3717
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6nj02087a2.cif
_cod_data_source_block           complex_2
_cod_depositor_comments
'Adding full bibliography for 7055807--7055811.cif.'
_cod_database_code               7055808
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.587
_shelx_estimated_absorpt_t_max   0.938
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu 0.40040(19) 0.81207(18) 0.17437(10) 0.0364(4) Uani 1 1 d . .
S1 S 0.7040(4) 0.6961(4) 0.1099(3) 0.0450(8) Uani 1 1 d . .
P1 P 0.0768(3) 0.7819(4) 0.3534(2) 0.0295(6) Uani 1 1 d . .
O1 O -0.0564(11) 0.7516(12) 0.4398(7) 0.047(2) Uani 1 1 d . .
N1 N 0.3138(13) 1.0294(12) 0.0710(8) 0.039(2) Uani 1 1 d . .
N2 N 0.3939(12) 0.8073(12) 0.3334(7) 0.0343(19) Uani 1 1 d . .
N3 N -0.0066(12) 1.1103(12) 0.2598(8) 0.037(2) Uani 1 1 d . .
N4 N 0.3045(12) 0.6226(11) 0.2066(7) 0.0317(18) Uani 1 1 d . .
C1 C 0.3069(13) 1.1462(14) -0.0043(9) 0.033(2) Uani 1 1 d . .
C2 C 0.5276(17) 0.8087(18) 0.3715(10) 0.046(3) Uani 1 1 d . .
H12 H 0.6250 0.8146 0.3247 0.055 Uiso 1 1 calc R U
C3 C 0.5299(19) 0.802(2) 0.4778(12) 0.064(4) Uani 1 1 d . .
H11 H 0.6280 0.7988 0.5024 0.077 Uiso 1 1 calc R U
C4 C 0.384(2) 0.799(3) 0.5452(11) 0.071(5) Uani 1 1 d . .
H1 H 0.3807 0.8008 0.6158 0.086 Uiso 1 1 calc R U
C5 C 0.2355(16) 0.7948(16) 0.5101(8) 0.039(3) Uani 1 1 d . .
H10 H 0.1358 0.7906 0.5552 0.047 Uiso 1 1 calc R U
C6 C 0.2540(13) 0.7973(14) 0.4014(8) 0.030(2) Uani 1 1 d . .
C7 C -0.0088(12) 0.9702(13) 0.2465(8) 0.028(2) Uani 1 1 d . .
C8 C -0.0854(16) 0.9704(15) 0.1625(9) 0.040(3) Uani 1 1 d . .
H2 H -0.0893 0.8712 0.1581 0.048 Uiso 1 1 calc R U
C9 C -0.1559(17) 1.1218(15) 0.0852(10) 0.044(3) Uani 1 1 d . .
H3 H -0.2070 1.1264 0.0273 0.053 Uiso 1 1 calc R U
C10 C -0.1487(16) 1.2647(16) 0.0961(10) 0.045(3) Uani 1 1 d . .
H4 H -0.1960 1.3684 0.0458 0.055 Uiso 1 1 calc R U
C11 C -0.0708(19) 1.2531(15) 0.1823(12) 0.052(3) Uani 1 1 d . .
H5 H -0.0625 1.3503 0.1868 0.062 Uiso 1 1 calc R U
C12 C 0.1833(13) 0.6092(14) 0.2894(8) 0.031(2) Uani 1 1 d . .
C13 C 0.3825(17) 0.4956(15) 0.1606(11) 0.045(3) Uani 1 1 d . .
H9 H 0.4654 0.5045 0.1028 0.054 Uiso 1 1 calc R U
C14 C 0.3445(19) 0.3476(17) 0.1962(12) 0.051(3) Uani 1 1 d . .
H8 H 0.4010 0.2611 0.1622 0.061 Uiso 1 1 calc R U
C15 C 0.225(2) 0.3338(16) 0.2803(12) 0.053(3) Uani 1 1 d . .
H7 H 0.1995 0.2366 0.3056 0.064 Uiso 1 1 calc R U
C16 C 0.1386(17) 0.4676(15) 0.3297(10) 0.042(3) Uani 1 1 d . .
H6 H 0.0548 0.4614 0.3872 0.050 Uiso 1 1 calc R U
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'
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
N1 Cu1 N4 125.4(4) . .
N1 Cu1 N2 118.1(4) . .
N4 Cu1 N2 95.9(4) . .
N1 Cu1 S1 102.1(3) . .
N4 Cu1 S1 106.5(3) . .
N2 Cu1 S1 107.8(3) . .
C1 S1 Cu1 96.1(4) 2_675 .
O1 P1 C7 114.3(5) . .
O1 P1 C6 112.6(5) . .
C7 P1 C6 106.7(5) . .
O1 P1 C12 112.2(5) . .
C7 P1 C12 105.5(5) . .
C6 P1 C12 104.9(5) . .
C1 N1 Cu1 161.9(9) . .
C2 N2 C6 118.2(10) . .
C2 N2 Cu1 121.6(8) . .
C6 N2 Cu1 120.2(7) . .
C11 N3 C7 116.4(10) . .
C13 N4 C12 118.2(10) . .
C13 N4 Cu1 121.1(8) . .
C12 N4 Cu1 119.5(7) . .
N1 C1 S1 178.3(11) . 2_675
N2 C2 C3 123.3(11) . .
N2 C2 H12 118.3 . .
C3 C2 H12 118.3 . .
C4 C3 C2 118.1(12) . .
C4 C3 H11 121.0 . .
C2 C3 H11 121.0 . .
C3 C4 C5 121.7(12) . .
C3 C4 H1 119.2 . .
C5 C4 H1 119.2 . .
C6 C5 C4 113.9(11) . .
C6 C5 H10 123.1 . .
C4 C5 H10 123.1 . .
N2 C6 C5 124.8(10) . .
N2 C6 P1 118.9(8) . .
C5 C6 P1 116.3(8) . .
N3 C7 C8 123.5(10) . .
N3 C7 P1 114.8(7) . .
C8 C7 P1 121.4(8) . .
C9 C8 C7 118.4(11) . .
C9 C8 H2 120.8 . .
C7 C8 H2 120.8 . .
C10 C9 C8 118.5(11) . .
C10 C9 H3 120.7 . .
C8 C9 H3 120.7 . .
C9 C10 C11 119.2(11) . .
C9 C10 H4 120.4 . .
C11 C10 H4 120.4 . .
N3 C11 C10 123.8(11) . .
N3 C11 H5 118.1 . .
C10 C11 H5 118.1 . .
N4 C12 C16 122.9(11) . .
N4 C12 P1 118.5(7) . .
C16 C12 P1 118.6(9) . .
N4 C13 C14 122.6(12) . .
N4 C13 H9 118.7 . .
C14 C13 H9 118.7 . .
C15 C14 C13 118.9(12) . .
C15 C14 H8 120.5 . .
C13 C14 H8 120.5 . .
C14 C15 C16 119.6(11) . .
C14 C15 H7 120.2 . .
C16 C15 H7 120.2 . .
C12 C16 C15 117.7(11) . .
C12 C16 H6 121.1 . .
C15 C16 H6 121.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.925(9) .
Cu1 N4 2.074(9) .
Cu1 N2 2.075(9) .
Cu1 S1 2.400(3) .
S1 C1 1.623(11) 2_675
P1 O1 1.472(8) .
P1 C7 1.795(10) .
P1 C6 1.799(10) .
P1 C12 1.821(12) .
N1 C1 1.181(14) .
N2 C2 1.323(15) .
N2 C6 1.343(13) .
N3 C11 1.334(15) .
N3 C7 1.340(14) .
N4 C13 1.330(15) .
N4 C12 1.346(13) .
C1 S1 1.623(11) 2_675
C2 C3 1.387(19) .
C2 H12 0.9300 .
C3 C4 1.37(2) .
C3 H11 0.9300 .
C4 C5 1.431(18) .
C4 H1 0.9300 .
C5 C6 1.405(14) .
C5 H10 0.9300 .
C7 C8 1.387(15) .
C8 C9 1.385(16) .
C8 H2 0.9300 .
C9 C10 1.369(18) .
C9 H3 0.9300 .
C10 C11 1.376(17) .
C10 H4 0.9300 .
C11 H5 0.9300 .
C12 C16 1.392(14) .
C13 C14 1.413(17) .
C13 H9 0.9300 .
C14 C15 1.35(2) .
C14 H8 0.9300 .
C15 C16 1.41(2) .
C15 H7 0.9300 .
C16 H6 0.9300 .
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
C16 H6 O1 0.93 2.46 3.171(14) 133.2 2_566
C11 H5 S1 0.93 2.87 3.516(13) 128.1 1_465
C3 H11 O1 0.93 2.50 3.256(16) 138.4 1_655
C16 H6 O1 0.93 2.46 3.171(14) 133.2 2_566
C11 H5 S1 0.93 2.87 3.516(13) 128.1 1_465
C3 H11 O1 0.93 2.50 3.256(16) 138.4 1_655
C16 H6 O1 0.93 2.46 3.171(14) 133.2 2_566
C11 H5 S1 0.93 2.87 3.516(13) 128.1 1_465
C3 H11 O1 0.93 2.50 3.256(16) 138.4 1_655
C16 H6 O1 0.93 2.46 3.171(14) 133.2 2_566
C11 H5 S1 0.93 2.87 3.516(13) 128.1 1_465
C3 H11 O1 0.93 2.50 3.256(16) 138.4 1_655
C16 H6 O1 0.93 2.46 3.171(14) 133.2 2_566
C11 H5 S1 0.93 2.87 3.516(13) 128.1 1_465
C3 H11 O1 0.93 2.50 3.256(16) 138.4 1_655
C3 H11 O1 0.93 2.50 3.256(16) 138.4 1_655
C11 H5 S1 0.93 2.87 3.516(13) 128.1 1_465
C16 H6 O1 0.93 2.46 3.171(14) 133.2 2_566
C3 H11 O1 0.93 2.50 3.256(16) 138.4 1_655
C11 H5 S1 0.93 2.87 3.516(13) 128.1 1_465
C16 H6 O1 0.93 2.46 3.171(14) 133.2 2_566
C3 H11 O1 0.93 2.50 3.256(16) 138.4 1_655
C11 H5 S1 0.93 2.87 3.516(13) 128.1 1_465
C16 H6 O1 0.93 2.46 3.171(14) 133.2 2_566
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C6 N2 C2 C3 -1(2)
Cu1 N2 C2 C3 -178.5(12)
N2 C2 C3 C4 -2(3)
C2 C3 C4 C5 3(3)
C3 C4 C5 C6 -1(2)
C2 N2 C6 C5 2.6(18)
Cu1 N2 C6 C5 -179.4(9)
C2 N2 C6 P1 -176.2(9)
Cu1 N2 C6 P1 1.8(12)
C4 C5 C6 N2 -1.6(19)
C4 C5 C6 P1 177.2(11)
O1 P1 C6 N2 173.2(9)
C7 P1 C6 N2 -60.7(10)
C12 P1 C6 N2 51.0(10)
O1 P1 C6 C5 -5.7(11)
C7 P1 C6 C5 120.4(9)
C12 P1 C6 C5 -127.9(9)
C11 N3 C7 C8 -5.2(17)
C11 N3 C7 P1 -179.4(10)
O1 P1 C7 N3 90.2(9)
C6 P1 C7 N3 -34.9(9)
C12 P1 C7 N3 -146.1(8)
O1 P1 C7 C8 -84.1(10)
C6 P1 C7 C8 150.8(9)
C12 P1 C7 C8 39.5(10)
N3 C7 C8 C9 3.3(17)
P1 C7 C8 C9 177.1(9)
C7 C8 C9 C10 -0.8(19)
C8 C9 C10 C11 1(2)
C7 N3 C11 C10 5(2)
C9 C10 C11 N3 -3(2)
C13 N4 C12 C16 1.0(16)
Cu1 N4 C12 C16 -166.7(8)
C13 N4 C12 P1 179.6(9)
Cu1 N4 C12 P1 11.9(11)
O1 P1 C12 N4 178.0(8)
C7 P1 C12 N4 53.0(9)
C6 P1 C12 N4 -59.5(9)
O1 P1 C12 C16 -3.4(10)
C7 P1 C12 C16 -128.4(9)
C6 P1 C12 C16 119.2(9)
C12 N4 C13 C14 -0.8(18)
Cu1 N4 C13 C14 166.8(10)
N4 C13 C14 C15 0(2)
C13 C14 C15 C16 1(2)
N4 C12 C16 C15 -0.3(17)
P1 C12 C16 C15 -178.9(9)
C14 C15 C16 C12 -0.7(19)
