#------------------------------------------------------------------------------
#$Date: 2019-12-26 22:26:51 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246185 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/19/2311957.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_2311957
loop_
_publ_author_name
'Fan, Le Qing'
'Zhu, Xiao Tong'
_publ_section_title
;
 Syntheses and crystal structures of two heterometallic iodoplumbates
 containing mixed-valence copper(I/II).
;
_journal_coeditor_code           OV3096
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              1098
_journal_page_last               1103
_journal_paper_doi               10.1107/S2053229617015807
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Cu2 Pb I5 (C12 H8 N2)2], 0.5I2'
_chemical_formula_moiety         'C24 H16 Cu2 I5 N4 Pb, 0.5(I2)'
_chemical_formula_sum            'C24 H16 Cu2 I6 N4 Pb'
_chemical_formula_weight         1456.08
_chemical_name_systematic
'Poly[[μ₃-iodido-tri-μ₂-iodido-iodido[bis(1,10-phenanthroline)copper(I)]copper(I)copper(II)lead(II)] hemiiodine]'
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 128.789(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5853(9)
_cell_length_b                   18.1041(8)
_cell_length_c                   13.0705(6)
_cell_measurement_reflns_used    3122
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1480
_cell_measurement_theta_min      3.3280
_cell_volume                     3243.5(3)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2007)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2007)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2007)
;
_computing_molecular_graphics
;
XP (Sheldrick, 1998)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'ω scans'
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7250
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         29.27
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrystalClear; Rigaku, 2007)
;
_exptl_crystal_colour            Gray
_exptl_crystal_density_diffrn    2.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.771
_refine_diff_density_min         -1.797
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0393
_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)+(0.0331P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                2846
_reflns_number_total             3837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ov3096sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2311957
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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
Pb Pb1 0.33381(3) 1.0000 0.24178(4) 0.04529(14) Uani d S 1 2
I I1 0.5000 0.88817(3) 0.5000 0.03561(17) Uani d S 1 2
I I2 0.44875(5) 1.0000 0.14749(8) 0.0531(2) Uani d S 1 2
I I3 0.19990(4) 1.12533(3) 0.05619(6) 0.05326(17) Uani d . 1 1
I I4 -0.08048(6) 1.0000 -0.20893(8) 0.0513(2) Uani d S 1 2
I I5 0.01894(7) 1.0000 0.41125(11) 0.0718(3) Uani d S 1 2
Cu Cu1 0.5000 0.73835(6) 0.5000 0.0327(3) Uani d S 1 2
Cu Cu2 0.0946(5) 1.0000 0.0131(6) 0.0640(14) Uani d SP 0.572(4) 2
Cu Cu2' 0.0734(8) 1.0360(5) 0.0133(9) 0.075(2) Uani d P 0.2141(19) 1
N N1 0.6309(4) 0.6825(3) 0.6218(6) 0.0343(14) Uani d . 1 1
N N2 0.5332(4) 0.7359(3) 0.3799(6) 0.0296(13) Uani d . 1 1
C C1 0.6774(6) 0.6545(4) 0.7410(8) 0.047(2) Uani d . 1 1
H H1A 0.6515 0.6626 0.7840 0.056 Uiso calc R 1 1
C C2 0.7613(6) 0.6145(5) 0.8040(10) 0.062(3) Uani d . 1 1
H H2A 0.7899 0.5949 0.8866 0.074 Uiso calc R 1 1
C C3 0.8035(6) 0.6031(4) 0.7460(9) 0.053(2) Uani d . 1 1
H H3A 0.8622 0.5776 0.7899 0.063 Uiso calc R 1 1
C C4 0.7564(5) 0.6305(4) 0.6189(9) 0.0430(19) Uani d . 1 1
C C5 0.6692(5) 0.6706(3) 0.5606(7) 0.0329(16) Uani d . 1 1
C C6 0.7914(6) 0.6217(4) 0.5450(10) 0.052(2) Uani d . 1 1
H H6A 0.8490 0.5958 0.5823 0.063 Uiso calc R 1 1
C C7 0.7432(6) 0.6500(4) 0.4241(9) 0.047(2) Uani d . 1 1
H H7A 0.7689 0.6444 0.3803 0.056 Uiso calc R 1 1
C C8 0.6524(6) 0.6889(4) 0.3608(8) 0.0412(18) Uani d . 1 1
C C9 0.6181(5) 0.6990(3) 0.4320(7) 0.0318(16) Uani d . 1 1
C C10 0.5990(6) 0.7187(4) 0.2374(9) 0.052(2) Uani d . 1 1
H H10A 0.6200 0.7128 0.1878 0.062 Uiso calc R 1 1
C C11 0.5156(6) 0.7569(4) 0.1869(8) 0.0460(19) Uani d . 1 1
H H11A 0.4795 0.7772 0.1032 0.055 Uiso calc R 1 1
C C12 0.4849(5) 0.7651(4) 0.2619(8) 0.0390(17) Uani d . 1 1
H H12A 0.4286 0.7921 0.2278 0.047 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
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'
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'
Pb Pb -3.3944 10.1111 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
I2 Pb1 I3 . 6_575 93.270(18)
I2 Pb1 I3 . . 93.270(18)
I3 Pb1 I3 6_575 . 95.33(3)
I2 Pb1 Cu2 . . 116.08(13)
I3 Pb1 Cu2 6_575 . 51.11(4)
I3 Pb1 Cu2 . . 51.11(4)
I2 Pb1 I1 . 5_676 91.531(17)
I3 Pb1 I1 6_575 5_676 167.623(18)
I3 Pb1 I1 . 5_676 95.777(16)
Cu2 Pb1 I1 . 5_676 135.34(7)
I2 Pb1 I1 . . 91.531(17)
I3 Pb1 I1 6_575 . 95.777(16)
I3 Pb1 I1 . . 167.623(18)
Cu2 Pb1 I1 . . 135.34(7)
I1 Pb1 I1 5_676 . 72.680(19)
Cu1 I1 Pb1 . 5_676 126.340(10)
Cu1 I1 Pb1 . . 126.340(10)
Pb1 I1 Pb1 5_676 . 107.320(19)
Cu2' I3 Cu2 . . 15.6(3)
Cu2' I3 Pb1 . . 80.5(2)
Cu2 I3 Pb1 . . 68.74(12)
Cu2' I4 Cu2' . 6_575 30.0(4)
Cu2' I4 Cu2' . 2 55.8(5)
Cu2' I4 Cu2' 6_575 2 64.5(5)
Cu2' I4 Cu2' . 5_575 64.5(5)
Cu2' I4 Cu2' 6_575 5_575 55.8(5)
Cu2' I4 Cu2' 2 5_575 29.5(4)
Cu2' I4 Cu2 . . 16.9(2)
Cu2' I4 Cu2 6_575 . 16.9(2)
Cu2' I4 Cu2 2 . 66.5(2)
Cu2' I4 Cu2 5_575 . 66.5(2)
Cu2' I4 Cu2 . 5_575 65.2(2)
Cu2' I4 Cu2 6_575 5_575 65.2(2)
Cu2' I4 Cu2 2 5_575 16.0(2)
Cu2' I4 Cu2 5_575 5_575 16.0(2)
Cu2 I4 Cu2 . 5_575 72.0(3)
N2 Cu1 N2 . 2_656 177.4(3)
N2 Cu1 N1 . 2_656 96.7(2)
N2 Cu1 N1 2_656 2_656 82.0(2)
N2 Cu1 N1 . . 82.0(2)
N2 Cu1 N1 2_656 . 96.7(2)
N1 Cu1 N1 2_656 . 121.4(3)
N2 Cu1 I1 . . 91.28(15)
N2 Cu1 I1 2_656 . 91.28(15)
N1 Cu1 I1 2_656 . 119.31(15)
N1 Cu1 I1 . . 119.31(16)
Cu2' Cu2 Cu2' . 6_575 120(3)
Cu2' Cu2 I4 . . 76.1(11)
Cu2' Cu2 I4 6_575 . 76.1(11)
Cu2' Cu2 I4 . 5_575 70.1(12)
Cu2' Cu2 I4 6_575 5_575 70.1(12)
I4 Cu2 I4 . 5_575 108.0(3)
Cu2' Cu2 Cu2' . 2 47.0(13)
Cu2' Cu2 Cu2' 6_575 2 73.6(14)
I4 Cu2 Cu2' . 2 56.3(2)
I4 Cu2 Cu2' 5_575 2 53.9(2)
Cu2' Cu2 Cu2' . 5_575 73.6(14)
Cu2' Cu2 Cu2' 6_575 5_575 47.0(13)
I4 Cu2 Cu2' . 5_575 56.3(2)
I4 Cu2 Cu2' 5_575 5_575 53.9(2)
Cu2' Cu2 Cu2' 2 5_575 26.7(4)
Cu2' Cu2 I3 . . 63.7(12)
Cu2' Cu2 I3 6_575 . 170.0(12)
I4 Cu2 I3 . . 113.83(15)
I4 Cu2 I3 5_575 . 104.68(16)
Cu2' Cu2 I3 2 . 110.62(16)
Cu2' Cu2 I3 5_575 . 137.1(3)
Cu2' Cu2 I3 . 6_575 170.0(12)
Cu2' Cu2 I3 6_575 6_575 63.7(12)
I4 Cu2 I3 . 6_575 113.83(15)
I4 Cu2 I3 5_575 6_575 104.68(16)
Cu2' Cu2 I3 2 6_575 137.1(3)
Cu2' Cu2 I3 5_575 6_575 110.62(16)
I3 Cu2 I3 . 6_575 110.9(3)
Cu2' Cu2 Pb1 . . 110.5(12)
Cu2' Cu2 Pb1 6_575 . 110.5(12)
I4 Cu2 Pb1 . . 164.1(3)
I4 Cu2 Pb1 5_575 . 87.93(17)
Cu2' Cu2 Pb1 2 . 138.83(16)
Cu2' Cu2 Pb1 5_575 . 138.83(16)
I3 Cu2 Pb1 . . 60.15(12)
I3 Cu2 Pb1 6_575 . 60.15(12)
Cu2 Cu2' Cu2' . 6_575 29.9(13)
Cu2 Cu2' Cu2' . 2 119.6(13)
Cu2' Cu2' Cu2' 6_575 2 90.000(5)
Cu2 Cu2' I4 . . 87.0(11)
Cu2' Cu2' I4 6_575 . 75.0(2)
Cu2' Cu2' I4 2 . 63.1(4)
Cu2 Cu2' I3 . . 100.8(14)
Cu2' Cu2' I3 6_575 . 130.0(2)
Cu2' Cu2' I3 2 . 139.5(2)
I4 Cu2' I3 . . 125.8(4)
Cu2 Cu2' I4 . 5_575 93.9(12)
Cu2' Cu2' I4 6_575 5_575 75.27(19)
Cu2' Cu2' I4 2 5_575 61.1(4)
I4 Cu2' I4 . 5_575 115.5(5)
I3 Cu2' I4 . 5_575 117.3(3)
Cu2 Cu2' Cu2' . 5_575 91.0(14)
Cu2' Cu2' Cu2' 6_575 5_575 61.3(4)
Cu2' Cu2' Cu2' 2 5_575 28.7(4)
I4 Cu2' Cu2' . 5_575 58.6(3)
I3 Cu2' Cu2' . 5_575 167.5(6)
I4 Cu2' Cu2' 5_575 5_575 56.9(4)
Cu2 Cu2' Cu2 . 5_575 106.4(14)
Cu2' Cu2' Cu2 6_575 5_575 76.66(19)
Cu2' Cu2' Cu2 2 5_575 13.37(18)
I4 Cu2' Cu2 . 5_575 60.9(3)
I3 Cu2' Cu2 . 5_575 152.5(4)
I4 Cu2' Cu2 5_575 5_575 57.2(2)
Cu2' Cu2' Cu2 5_575 5_575 15.4(2)
C1 N1 C5 . . 117.7(6)
C1 N1 Cu1 . . 131.6(5)
C5 N1 Cu1 . . 110.6(5)
C12 N2 C9 . . 118.8(6)
C12 N2 Cu1 . . 128.4(5)
C9 N2 Cu1 . . 112.8(5)
N1 C1 C2 . . 123.5(8)
N1 C1 H1A . . 118.2
C2 C1 H1A . . 118.2
C1 C2 C3 . . 120.2(9)
C1 C2 H2A . . 119.9
C3 C2 H2A . . 119.9
C2 C3 C4 . . 118.7(7)
C2 C3 H3A . . 120.6
C4 C3 H3A . . 120.6
C3 C4 C5 . . 117.2(7)
C3 C4 C6 . . 124.8(7)
C5 C4 C6 . . 118.0(8)
N1 C5 C4 . . 122.7(7)
N1 C5 C9 . . 117.7(6)
C4 C5 C9 . . 119.7(7)
C7 C6 C4 . . 121.8(7)
C7 C6 H6A . . 119.1
C4 C6 H6A . . 119.1
C6 C7 C8 . . 121.2(7)
C6 C7 H7A . . 119.4
C8 C7 H7A . . 119.4
C10 C8 C9 . . 117.9(7)
C10 C8 C7 . . 124.3(7)
C9 C8 C7 . . 117.8(8)
N2 C9 C8 . . 121.5(7)
N2 C9 C5 . . 116.9(6)
C8 C9 C5 . . 121.5(6)
C11 C10 C8 . . 120.4(7)
C11 C10 H10A . . 119.8
C8 C10 H10A . . 119.8
C10 C11 C12 . . 119.3(8)
C10 C11 H11A . . 120.4
C12 C11 H11A . . 120.4
N2 C12 C11 . . 122.0(7)
N2 C12 H12A . . 119.0
C11 C12 H12A . . 119.0
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
Pb1 I2 . 2.9538(9) yes
Pb1 I3 6_575 3.0693(6) yes
Pb1 I3 . 3.0693(6) yes
Pb1 Cu2 . 3.298(7) ?
Pb1 I1 5_676 3.4165(5) yes
Pb1 I1 . 3.4165(5) yes
I1 Cu1 . 2.7124(13) yes
I1 Pb1 5_676 3.4165(5) ?
I3 Cu2' . 2.513(12) ?
I3 Cu2 . 2.755(4) yes
I4 Cu2' . 2.517(10) ?
I4 Cu2' 6_575 2.517(10) ?
I4 Cu2' 2 2.565(10) ?
I4 Cu2' 5_575 2.565(10) ?
I4 Cu2 . 2.590(6) ?
I4 Cu2 5_575 2.722(7) yes
I5 I5 5_576 2.786(2) ?
Cu1 N2 . 1.988(5) yes
Cu1 N2 2_656 1.988(5) yes
Cu1 N1 2_656 2.064(6) yes
Cu1 N1 . 2.064(6) yes
Cu2 Cu2' . 0.752(9) ?
Cu2 Cu2' 6_575 0.752(9) ?
Cu2 I4 5_575 2.722(7) yes
Cu2 Cu2' 2 2.827(8) ?
Cu2 Cu2' 5_575 2.827(8) ?
Cu2 I3 6_575 2.755(4) yes
Cu2' Cu2' 6_575 1.305(18) ?
Cu2' Cu2' 2 2.38(2) ?
Cu2' I4 5_575 2.565(10) ?
Cu2' Cu2' 5_575 2.71(2) ?
Cu2' Cu2 5_575 2.827(8) ?
N1 C1 . 1.325(9) ?
N1 C5 . 1.350(8) ?
N2 C12 . 1.319(9) ?
N2 C9 . 1.366(8) ?
C1 C2 . 1.362(10) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.368(11) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.403(11) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.412(9) ?
C4 C6 . 1.442(11) ?
C5 C9 . 1.415(10) ?
C6 C7 . 1.342(11) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.441(10) ?
C7 H7A . 0.9300 ?
C8 C10 . 1.370(11) ?
C8 C9 . 1.402(9) ?
C10 C11 . 1.361(11) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.393(10) ?
C11 H11A . 0.9300 ?
C12 H12A . 0.9300 ?
