#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:39:07 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224304 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/83/7048352.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_7048352
loop_
_publ_author_name
'Artem'ev, Alexander V.'
'Pritchina, Elena A.'
'Rakhmanova, Marianna I.'
'Gritsan, Nina P.'
'Bagryanskaya, Irina Yu'
'Malysheva, Svetlana F.'
'Belogorlova, Nataliya A.'
_publ_section_title
;
 Alkyl-dependent self-assembly of the first red-emitting zwitterionic
 {Cu₄I₆} clusters from
 [alkyl-P(2-Py)₃]⁺ salts and CuI: when size matters.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2328
_journal_page_last               2337
_journal_paper_doi               10.1039/c8dt04328k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C44 H38 Cu4 I6 N6 P2'
_chemical_formula_sum            'C44 H38 Cu4 I6 N6 P2'
_chemical_formula_weight         1728.30
_chemical_name_systematic
;
 complex of copper(I) iodide with benzyltri(pyridin-2-yl)phosphonium iodide
;
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-13 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                118.947(2)
_cell_angle_beta                 92.187(2)
_cell_angle_gamma                107.225(2)
_cell_formula_units_Z            1
_cell_length_a                   10.1053(4)
_cell_length_b                   12.2864(5)
_cell_length_c                   12.3397(6)
_cell_measurement_reflns_used    9296
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      2.37
_cell_volume                     1249.98(10)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_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  0.0334
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35481
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.568
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.485
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_correction_T_min  0.4877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.372
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0398P)²+4.2204P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4772
_reflns_number_total             5118
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04328k2.cif
_cod_data_source_block           complex_4_q6
_cod_depositor_comments
'Adding full bibliography for 7048350--7048353.cif.'
_cod_database_code               7048352
_shelx_shelxl_version_number     2014/7
_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   0.218
_shelx_estimated_absorpt_t_max   0.407
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
I3 I 0.19039(3) 0.58817(3) 0.62584(3) 0.04135(9) Uani 1 1 d . .
Cu1 Cu 0.28491(6) 0.61905(5) 0.27458(5) 0.03596(13) Uani 1 1 d . .
I1 I 0.12015(3) 0.74944(3) 0.37099(3) 0.04196(9) Uani 1 1 d . .
P1 P 0.57038(10) 0.82532(9) 0.25099(9) 0.02395(19) Uani 1 1 d . .
N1 N 0.4918(4) 0.7038(3) 0.3821(3) 0.0302(7) Uani 1 1 d . .
I2 I 0.18483(3) 0.36972(3) 0.21399(3) 0.04238(9) Uani 1 1 d . .
Cu2 Cu 0.08341(7) 0.53234(7) 0.39789(7) 0.05315(17) Uani 1 1 d . .
N2 N 0.3391(3) 0.6092(3) 0.1080(3) 0.0280(7) Uani 1 1 d . .
N3 N 0.8062(4) 0.8235(4) 0.1693(4) 0.0427(9) Uani 1 1 d . .
C1 C 0.5145(5) 0.6632(5) 0.4618(4) 0.0411(10) Uani 1 1 d . .
H1A H 0.4366 0.6151 0.4784 0.049 Uiso 1 1 calc R U
C2 C 0.6488(6) 0.6896(6) 0.5201(5) 0.0490(12) Uani 1 1 d . .
H2 H 0.6606 0.6589 0.5741 0.059 Uiso 1 1 calc R U
C3 C 0.7635(6) 0.7611(6) 0.4980(5) 0.0536(13) Uani 1 1 d . .
H3 H 0.8547 0.7792 0.5363 0.064 Uiso 1 1 calc R U
C4 C 0.7436(5) 0.8067(5) 0.4180(4) 0.0430(10) Uani 1 1 d . .
H4A H 0.8207 0.8569 0.4025 0.052 Uiso 1 1 calc R U
C5 C 0.6066(4) 0.7757(4) 0.3621(3) 0.0263(7) Uani 1 1 d . .
C6 C 0.4644(4) 0.6810(4) 0.1000(4) 0.0252(7) Uani 1 1 d . .
C7 C 0.5031(5) 0.6569(4) -0.0131(4) 0.0333(8) Uani 1 1 d . .
H7 H 0.5931 0.7049 -0.0141 0.040 Uiso 1 1 calc R U
C8 C 0.4052(5) 0.5596(5) -0.1251(4) 0.0402(10) Uani 1 1 d . .
H8 H 0.4275 0.5424 -0.2029 0.048 Uiso 1 1 calc R U
C9 C 0.2742(5) 0.4887(4) -0.1195(4) 0.0418(10) Uani 1 1 d . .
H9 H 0.2056 0.4247 -0.1934 0.050 Uiso 1 1 calc R U
C10 C 0.2462(5) 0.5139(4) -0.0021(4) 0.0376(9) Uani 1 1 d . .
H10 H 0.1592 0.4627 0.0006 0.045 Uiso 1 1 calc R U
C11 C 0.7382(4) 0.9066(4) 0.2289(4) 0.0283(8) Uani 1 1 d . .
C15 C 0.7909(4) 1.0414(4) 0.2739(4) 0.0348(9) Uani 1 1 d . .
H15A H 0.7404 1.0957 0.3168 0.042 Uiso 1 1 calc R U
C12 C 0.9232(5) 1.0932(5) 0.2525(5) 0.0433(10) Uani 1 1 d . .
H12 H 0.9627 1.1833 0.2799 0.052 Uiso 1 1 calc R U
C13 C 0.9931(5) 1.0101(5) 0.1911(5) 0.0502(12) Uani 1 1 d . .
H13 H 1.0809 1.0426 0.1751 0.060 Uiso 1 1 calc R U
C14 C 0.9331(5) 0.8768(5) 0.1522(5) 0.0519(13) Uani 1 1 d . .
H14 H 0.9838 0.8217 0.1123 0.062 Uiso 1 1 calc R U
C16 C 0.4702(4) 0.9350(4) 0.3128(4) 0.0296(8) Uani 1 1 d . .
H16B H 0.3897 0.8937 0.3379 0.036 Uiso 1 1 calc R U
H16A H 0.5299 1.0178 0.3880 0.036 Uiso 1 1 calc R U
C17 C 0.4166(4) 0.9662(4) 0.2187(4) 0.0284(8) Uani 1 1 d . .
C18 C 0.3032(5) 0.8739(5) 0.1172(5) 0.0415(10) Uani 1 1 d . .
H18 H 0.2564 0.7911 0.1073 0.050 Uiso 1 1 calc R U
C19 C 0.2586(6) 0.9027(6) 0.0306(5) 0.0527(13) Uani 1 1 d . .
H19 H 0.1850 0.8384 -0.0393 0.063 Uiso 1 1 calc R U
C20 C 0.3245(6) 1.0286(6) 0.0482(6) 0.0565(14) Uani 1 1 d . .
H20 H 0.2949 1.0491 -0.0097 0.068 Uiso 1 1 calc R U
C21 C 0.4330(6) 1.1220(6) 0.1509(6) 0.0591(15) Uani 1 1 d . .
H21 H 0.4754 1.2069 0.1641 0.071 Uiso 1 1 calc R U
C22 C 0.4799(5) 1.0912(5) 0.2352(5) 0.0416(10) Uani 1 1 d . .
H22 H 0.5549 1.1551 0.3040 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'
P P 0.1023 0.0942 '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'
I I -0.4742 1.8119 '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
Cu2 I3 Cu2 78.72(2) . 2_566
N1 Cu1 N2 97.21(13) . .
N1 Cu1 I1 115.87(10) . .
N2 Cu1 I1 115.83(9) . .
N1 Cu1 I2 107.34(10) . .
N2 Cu1 I2 104.09(9) . .
I1 Cu1 I2 114.53(2) . .
N1 Cu1 Cu2 111.26(9) . .
N2 Cu1 Cu2 149.74(9) . .
I1 Cu1 Cu2 61.02(2) . .
I2 Cu1 Cu2 58.570(19) . .
Cu1 I1 Cu2 64.361(19) . .
C11 P1 C5 107.65(18) . .
C11 P1 C16 111.68(19) . .
C5 P1 C16 109.59(18) . .
C11 P1 C6 109.60(18) . .
C5 P1 C6 110.61(17) . .
C16 P1 C6 107.72(18) . .
C1 N1 C5 117.3(4) . .
C1 N1 Cu1 116.2(3) . .
C5 N1 Cu1 125.4(3) . .
Cu1 I2 Cu2 65.02(2) . .
I3 Cu2 I3 101.28(2) . 2_566
I3 Cu2 I2 112.84(3) . .
I3 Cu2 I2 110.92(3) 2_566 .
I3 Cu2 I1 115.74(3) . .
I3 Cu2 I1 109.30(3) 2_566 .
I2 Cu2 I1 106.71(2) . .
I3 Cu2 Cu1 115.13(3) . .
I3 Cu2 Cu1 143.59(3) 2_566 .
I2 Cu2 Cu1 56.413(18) . .
I1 Cu2 Cu1 54.622(18) . .
C10 N2 C6 116.7(3) . .
C10 N2 Cu1 117.0(3) . .
C6 N2 Cu1 125.9(3) . .
C14 N3 C11 116.5(4) . .
N1 C1 C2 122.7(4) . .
N1 C1 H1A 118.7 . .
C2 C1 H1A 118.7 . .
C3 C2 C1 119.3(4) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
C2 C3 C4 119.5(4) . .
C2 C3 H3 120.3 . .
C4 C3 H3 120.3 . .
C5 C4 C3 118.2(4) . .
C5 C4 H4A 120.9 . .
C3 C4 H4A 120.9 . .
N1 C5 C4 123.1(4) . .
N1 C5 P1 115.6(3) . .
C4 C5 P1 121.3(3) . .
N2 C6 C7 123.7(4) . .
N2 C6 P1 114.0(3) . .
C7 C6 P1 122.0(3) . .
C6 C7 C8 118.6(4) . .
C6 C7 H7 120.7 . .
C8 C7 H7 120.7 . .
C9 C8 C7 118.9(4) . .
C9 C8 H8 120.6 . .
C7 C8 H8 120.6 . .
C8 C9 C10 119.1(4) . .
C8 C9 H9 120.5 . .
C10 C9 H9 120.5 . .
N2 C10 C9 122.9(4) . .
N2 C10 H10 118.5 . .
C9 C10 H10 118.5 . .
N3 C11 C15 124.6(4) . .
N3 C11 P1 112.8(3) . .
C15 C11 P1 122.6(3) . .
C11 C15 C12 117.2(4) . .
C11 C15 H15A 121.4 . .
C12 C15 H15A 121.4 . .
C13 C12 C15 119.0(4) . .
C13 C12 H12 120.5 . .
C15 C12 H12 120.5 . .
C12 C13 C14 119.6(4) . .
C12 C13 H13 120.2 . .
C14 C13 H13 120.2 . .
N3 C14 C13 123.1(5) . .
N3 C14 H14 118.4 . .
C13 C14 H14 118.4 . .
C17 C16 P1 113.5(3) . .
C17 C16 H16B 108.9 . .
P1 C16 H16B 108.9 . .
C17 C16 H16A 108.9 . .
P1 C16 H16A 108.9 . .
H16B C16 H16A 107.7 . .
C18 C17 C22 118.4(4) . .
C18 C17 C16 121.9(4) . .
C22 C17 C16 119.7(4) . .
C19 C18 C17 121.1(5) . .
C19 C18 H18 119.5 . .
C17 C18 H18 119.5 . .
C18 C19 C20 119.6(5) . .
C18 C19 H19 120.2 . .
C20 C19 H19 120.2 . .
C21 C20 C19 119.6(5) . .
C21 C20 H20 120.2 . .
C19 C20 H20 120.2 . .
C20 C21 C22 120.4(5) . .
C20 C21 H21 119.8 . .
C22 C21 H21 119.8 . .
C21 C22 C17 120.7(5) . .
C21 C22 H22 119.6 . .
C17 C22 H22 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I3 Cu2 2.6481(8) .
I3 Cu2 2.6507(7) 2_566
Cu1 N1 2.092(3) .
Cu1 N2 2.104(3) .
Cu1 I1 2.5767(6) .
Cu1 I2 2.6185(6) .
Cu1 Cu2 2.8491(8) .
I1 Cu2 2.7645(8) .
P1 C11 1.800(4) .
P1 C5 1.814(4) .
P1 C16 1.815(4) .
P1 C6 1.813(4) .
N1 C1 1.340(5) .
N1 C5 1.347(5) .
I2 Cu2 2.6820(8) .
Cu2 I3 2.6506(7) 2_566
N2 C10 1.345(5) .
N2 C6 1.351(5) .
N3 C14 1.332(6) .
N3 C11 1.335(6) .
C1 C2 1.380(7) .
C1 H1A 0.9300 .
C2 C3 1.357(8) .
C2 H2 0.9300 .
C3 C4 1.384(7) .
C3 H3 0.9300 .
C4 C5 1.378(6) .
C4 H4A 0.9300 .
C6 C7 1.377(5) .
C7 C8 1.384(6) .
C7 H7 0.9300 .
C8 C9 1.378(7) .
C8 H8 0.9300 .
C9 C10 1.387(7) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C15 1.379(6) .
C15 C12 1.396(6) .
C15 H15A 0.9300 .
C12 C13 1.354(8) .
C12 H12 0.9300 .
C13 C14 1.382(7) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C16 C17 1.514(5) .
C16 H16B 0.9700 .
C16 H16A 0.9700 .
C17 C18 1.383(6) .
C17 C22 1.383(6) .
C18 C19 1.376(7) .
C18 H18 0.9300 .
C19 C20 1.393(8) .
C19 H19 0.9300 .
C20 C21 1.366(9) .
C20 H20 0.9300 .
C21 C22 1.378(7) .
C21 H21 0.9300 .
C22 H22 0.9300 .
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
C5 N1 C1 C2 -1.5(7)
Cu1 N1 C1 C2 167.2(4)
N1 C1 C2 C3 0.8(8)
C1 C2 C3 C4 0.4(9)
C2 C3 C4 C5 -0.9(8)
C1 N1 C5 C4 0.9(6)
Cu1 N1 C5 C4 -166.6(3)
C1 N1 C5 P1 178.8(3)
Cu1 N1 C5 P1 11.3(4)
C3 C4 C5 N1 0.3(7)
C3 C4 C5 P1 -177.5(4)
C11 P1 C5 N1 -175.0(3)
C16 P1 C5 N1 63.3(3)
C6 P1 C5 N1 -55.3(3)
C11 P1 C5 C4 2.9(4)
C16 P1 C5 C4 -118.8(4)
C6 P1 C5 C4 122.6(4)
C10 N2 C6 C7 -3.4(6)
Cu1 N2 C6 C7 169.6(3)
C10 N2 C6 P1 169.7(3)
Cu1 N2 C6 P1 -17.2(4)
C11 P1 C6 N2 176.7(3)
C5 P1 C6 N2 58.2(3)
C16 P1 C6 N2 -61.6(3)
C11 P1 C6 C7 -10.0(4)
C5 P1 C6 C7 -128.6(3)
C16 P1 C6 C7 111.7(3)
N2 C6 C7 C8 4.4(6)
P1 C6 C7 C8 -168.2(3)
C6 C7 C8 C9 -1.4(7)
C7 C8 C9 C10 -2.0(7)
C6 N2 C10 C9 -0.3(6)
Cu1 N2 C10 C9 -174.0(4)
C8 C9 C10 N2 3.0(7)
C14 N3 C11 C15 -0.7(7)
C14 N3 C11 P1 -178.3(4)
C5 P1 C11 N3 67.3(4)
C16 P1 C11 N3 -172.3(3)
C6 P1 C11 N3 -53.0(4)
C5 P1 C11 C15 -110.4(4)
C16 P1 C11 C15 9.9(4)
C6 P1 C11 C15 129.2(4)
N3 C11 C15 C12 1.7(7)
P1 C11 C15 C12 179.1(3)
C11 C15 C12 C13 -0.9(7)
C15 C12 C13 C14 -0.7(8)
C11 N3 C14 C13 -1.1(8)
C12 C13 C14 N3 1.8(9)
C11 P1 C16 C17 69.0(3)
C5 P1 C16 C17 -171.8(3)
C6 P1 C16 C17 -51.4(3)
P1 C16 C17 C18 74.7(4)
P1 C16 C17 C22 -106.7(4)
C22 C17 C18 C19 3.4(7)
C16 C17 C18 C19 -178.1(4)
C17 C18 C19 C20 -2.8(8)
C18 C19 C20 C21 0.3(9)
C19 C20 C21 C22 1.7(9)
C20 C21 C22 C17 -1.1(9)
C18 C17 C22 C21 -1.4(7)
C16 C17 C22 C21 -180.0(5)
