#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:09:46 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180468 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/37/7213767.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_7213767
loop_
_publ_author_name
'Zhang, Zhu-Yan'
'Deng, Zhao-Peng'
'Zhang, Xian-Fa'
'Huo, Li-Hua'
'Zhao, Hui'
'Gao, Shan'
_publ_section_title
;
 Self-assembly of [Cu3I2]- or [CuI]n-based (n = 2, 4, and ∞ )
 coordination polymers from unsymmetrical bis(pyridyl) and in situ
 ligands: syntheses, structures, and properties
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              359
_journal_paper_doi               10.1039/c3ce41774c
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'Cu3 I2 (C4 H6 N3) (C18 H15 P)2, C2 H3 N'
_chemical_formula_sum            'C42 H39 Cu3 I2 N4 P2'
_chemical_formula_weight         1106.13
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.0737(14)
_cell_length_b                   11.5118(7)
_cell_length_c                   16.6416(9)
_cell_measurement_reflns_used    18478
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      3.02
_cell_volume                     4420.3(4)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_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  0.0797
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40867
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.932
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         5038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0510
_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)+(0.0710P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                3002
_reflns_number_total             5038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41774c.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P ccn'
_cod_database_code               7213767
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
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
I1 I 0.698243(19) 0.90553(3) 0.20636(2) 0.06636(19) Uani 1 1 d .
Cu1 Cu 0.69470(4) 0.67658(7) 0.14223(4) 0.0718(3) Uani 1 1 d .
Cu2 Cu 0.7500 0.7500 0.29044(5) 0.0660(3) Uani 1 2 d S
P1 P 0.62159(7) 0.57420(13) 0.18785(9) 0.0600(4) Uani 1 1 d .
N1 N 0.7500 0.7500 0.4077(3) 0.0563(16) Uani 1 2 d S
N2 N 0.7249(2) 0.7833(4) 0.5359(2) 0.0628(12) Uani 1 1 d .
C1 C 0.55303(19) 0.6246(4) 0.1461(3) 0.0742(17) Uani 1 1 d G
C2 C 0.5098(3) 0.5489(4) 0.1207(4) 0.163(5) Uani 1 1 d G
H2 H 0.5156 0.4691 0.1237 0.210 Uiso 1 1 calc R
C3 C 0.4580(2) 0.5925(7) 0.0908(5) 0.164(5) Uani 1 1 d G
H3 H 0.4291 0.5418 0.0738 0.287 Uiso 1 1 calc R
C4 C 0.4493(2) 0.7118(7) 0.0862(4) 0.160(5) Uani 1 1 d G
H4 H 0.4146 0.7409 0.0662 0.193 Uiso 1 1 calc R
C5 C 0.4925(3) 0.7875(5) 0.1116(3) 0.117(3) Uani 1 1 d G
H5 H 0.4867 0.8673 0.1086 0.140 Uiso 1 1 calc R
C6 C 0.5444(2) 0.7439(4) 0.1415(3) 0.100(2) Uani 1 1 d G
H6 H 0.5733 0.7946 0.1585 0.120 Uiso 1 1 calc R
C7 C 0.6253(2) 0.4208(3) 0.1627(2) 0.0711(17) Uani 1 1 d G
C8 C 0.5942(2) 0.3366(4) 0.2044(3) 0.101(3) Uani 1 1 d G
H8 H 0.5710 0.3578 0.2476 0.122 Uiso 1 1 calc R
C9 C 0.5979(3) 0.2208(4) 0.1814(4) 0.117(3) Uani 1 1 d G
H9 H 0.5771 0.1645 0.2092 0.140 Uiso 1 1 calc R
C10 C 0.6327(3) 0.1891(3) 0.1168(4) 0.112(3) Uani 1 1 d G
H10 H 0.6351 0.1116 0.1014 0.134 Uiso 1 1 calc R
C11 C 0.6638(2) 0.2732(5) 0.0752(3) 0.103(3) Uani 1 1 d G
H11 H 0.6870 0.2520 0.0320 0.124 Uiso 1 1 calc R
C12 C 0.66007(19) 0.3891(4) 0.0982(2) 0.0767(18) Uani 1 1 d G
H12 H 0.6809 0.4454 0.0703 0.092 Uiso 1 1 calc R
C13 C 0.61036(19) 0.5739(4) 0.29757(17) 0.0661(16) Uani 1 1 d G
C14 C 0.56003(17) 0.6166(4) 0.3327(3) 0.091(2) Uani 1 1 d G
H14 H 0.5304 0.6458 0.3006 0.109 Uiso 1 1 calc R
C15 C 0.5540(2) 0.6157(5) 0.4158(3) 0.115(3) Uani 1 1 d G
H15 H 0.5203 0.6443 0.4393 0.138 Uiso 1 1 calc R
C16 C 0.5983(3) 0.5722(5) 0.46377(17) 0.106(3) Uani 1 1 d G
H16 H 0.5942 0.5716 0.5194 0.128 Uiso 1 1 calc R
C17 C 0.6486(2) 0.5295(4) 0.4286(2) 0.093(2) Uani 1 1 d G
H17 H 0.6782 0.5003 0.4607 0.112 Uiso 1 1 calc R
C18 C 0.65464(16) 0.5304(4) 0.3455(2) 0.0782(18) Uani 1 1 d G
H18 H 0.6883 0.5018 0.3220 0.094 Uiso 1 1 calc R
C19 C 0.7111(3) 0.8002(5) 0.4588(3) 0.0584(14) Uani 1 1 d .
C20 C 0.6604(3) 0.8686(6) 0.4332(3) 0.0771(19) Uani 1 1 d .
H20A H 0.6330 0.8730 0.4765 0.116 Uiso 1 1 calc R
H20B H 0.6425 0.8318 0.3877 0.116 Uiso 1 1 calc R
H20C H 0.6725 0.9455 0.4186 0.116 Uiso 1 1 calc R
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 I1 Cu1 64.64(2) . .
Cu2 I1 Cu1 64.52(2) . 2_665
Cu1 I1 Cu1 65.00(3) . 2_665
N2 Cu1 P1 135.54(1) 7_575 .
N2 Cu1 I1 96.33(14) 7_575 .
P1 Cu1 I1 112.96(5) . .
N2 Cu1 I1 96.20(2) 7_575 2_665
P1 Cu1 I1 111.01(5) . 2_665
I1 Cu1 I1 98.15(3) . 2_665
N2 Cu1 Cu2 122.88(14) 7_575 .
P1 Cu1 Cu2 101.56(5) . .
I1 Cu1 Cu2 53.046(16) . .
I1 Cu1 Cu2 52.976(16) 2_665 .
N1 Cu2 I1 123.029(18) . .
N1 Cu2 I1 123.029(18) . 2_665
I1 Cu2 I1 113.94(4) . 2_665
N1 Cu2 Cu1 148.181(16) . .
I1 Cu2 Cu1 62.32(2) . .
I1 Cu2 Cu1 62.50(3) 2_665 .
N1 Cu2 Cu1 148.181(16) . 2_665
I1 Cu2 Cu1 62.50(3) . 2_665
I1 Cu2 Cu1 62.32(2) 2_665 2_665
Cu1 Cu2 Cu1 63.64(3) . 2_665
C7 P1 C1 105.2(2) . .
C7 P1 C13 103.5(2) . .
C1 P1 C13 104.9(2) . .
C7 P1 Cu1 113.98(16) . .
C1 P1 Cu1 111.36(19) . .
C13 P1 Cu1 116.85(16) . .
C19 N1 C19 102.9(6) 2_665 .
C19 N1 Cu2 128.5(3) 2_665 .
C19 N1 Cu2 128.5(3) . .
C19 N2 N2 106.2(3) . 2_665
C19 N2 Cu1 138.5(4) . 7_576
N2 N2 Cu1 115.30(13) 2_665 7_576
C2 C1 C6 120.0 . .
C2 C1 P1 122.6(3) . .
C6 C1 P1 117.4(3) . .
C1 C2 C3 120.0 . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C4 C3 C2 120.0 . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C3 C4 C5 120.0 . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
C4 C5 C6 120.0 . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C5 C6 C1 120.0 . .
C5 C6 H6 120.0 . .
C1 C6 H6 120.0 . .
C8 C7 C12 120.0 . .
C8 C7 P1 122.6(3) . .
C12 C7 P1 117.4(3) . .
C7 C8 C9 120.0 . .
C7 C8 H8 120.0 . .
C9 C8 H8 120.0 . .
C10 C9 C8 120.0 . .
C10 C9 H9 120.0 . .
C8 C9 H9 120.0 . .
C9 C10 C11 120.0 . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C12 C11 C10 120.0 . .
C12 C11 H11 120.0 . .
C10 C11 H11 120.0 . .
C11 C12 C7 120.0 . .
C11 C12 H12 120.0 . .
C7 C12 H12 120.0 . .
C14 C13 C18 120.0 . .
C14 C13 P1 122.2(2) . .
C18 C13 P1 117.8(2) . .
C15 C14 C13 120.0 . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C14 C15 C16 120.0 . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
C15 C16 C17 120.0 . .
C15 C16 H16 120.0 . .
C17 C16 H16 120.0 . .
C16 C17 C18 120.0 . .
C16 C17 H17 120.0 . .
C18 C17 H17 120.0 . .
C17 C18 C13 120.0 . .
C17 C18 H18 120.0 . .
C13 C18 H18 120.0 . .
N2 C19 N1 112.3(5) . .
N2 C19 C20 123.0(5) . .
N1 C19 C20 124.6(4) . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Cu2 2.5671(6) .
I1 Cu1 2.8447(9) .
I1 Cu1 2.8520(6) 2_665
Cu1 N2 1.958(4) 7_575
Cu1 P1 2.1934(5) .
Cu1 I1 2.8520(6) 2_665
Cu1 Cu2 2.9027(6) .
Cu2 N1 1.952(5) .
Cu2 I1 2.5671(6) 2_665
Cu2 Cu1 2.9027(6) 2_665
P1 C7 1.817(4) .
P1 C1 1.823(4) .
P1 C13 1.844(3) .
N1 C19 1.364(6) 2_665
N1 C19 1.364(6) .
N2 C19 1.336(6) .
N2 N2 1.387(9) 2_665
N2 Cu1 1.958(4) 7_576
C1 C2 1.3900 .
C1 C6 1.3900 .
C2 C3 1.3900 .
C2 H2 0.9300 .
C3 C4 1.3900 .
C3 H3 0.9300 .
C4 C5 1.3900 .
C4 H4 0.9300 .
C5 C6 1.3900 .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.3900 .
C7 C12 1.3900 .
C8 C9 1.3900 .
C8 H8 0.9300 .
C9 C10 1.3900 .
C9 H9 0.9300 .
C10 C11 1.3900 .
C10 H10 0.9300 .
C11 C12 1.3900 .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 C14 1.3900 .
C13 C18 1.3900 .
C14 C15 1.3900 .
C14 H14 0.9300 .
C15 C16 1.3900 .
C15 H15 0.9300 .
C16 C17 1.3900 .
C16 H16 0.9300 .
C17 C18 1.3900 .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 C20 1.474(8) .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Cu2 I1 Cu1 N2 -126.87(16) . 7_575
Cu1 I1 Cu1 N2 -54.58(15) 2_665 7_575
Cu2 I1 Cu1 P1 87.34(5) . .
Cu1 I1 Cu1 P1 159.64(6) 2_665 .
Cu2 I1 Cu1 I1 -29.656(19) . 2_665
Cu1 I1 Cu1 I1 42.64(3) 2_665 2_665
Cu1 I1 Cu1 Cu2 72.29(2) 2_665 .
Cu1 I1 Cu2 N1 -143.460(18) . .
Cu1 I1 Cu2 N1 143.530(17) 2_665 .
Cu1 I1 Cu2 I1 36.540(17) . 2_665
Cu1 I1 Cu2 I1 -36.470(17) 2_665 2_665
Cu1 I1 Cu2 Cu1 -73.01(3) 2_665 .
Cu1 I1 Cu2 Cu1 73.01(3) . 2_665
N2 Cu1 Cu2 N1 180.00(19) 7_575 .
P1 Cu1 Cu2 N1 -1.36(7) . .
I1 Cu1 Cu2 N1 108.78(3) . .
I1 Cu1 Cu2 N1 -109.06(3) 2_665 .
N2 Cu1 Cu2 I1 71.22(19) 7_575 .
P1 Cu1 Cu2 I1 -110.14(5) . .
I1 Cu1 Cu2 I1 142.16(2) 2_665 .
N2 Cu1 Cu2 I1 -70.94(19) 7_575 2_665
P1 Cu1 Cu2 I1 107.70(5) . 2_665
I1 Cu1 Cu2 I1 -142.16(2) . 2_665
N2 Cu1 Cu2 Cu1 0.00(19) 7_575 2_665
P1 Cu1 Cu2 Cu1 178.64(7) . 2_665
I1 Cu1 Cu2 Cu1 -71.22(3) . 2_665
I1 Cu1 Cu2 Cu1 70.94(3) 2_665 2_665
N2 Cu1 P1 C7 63.5(3) 7_575 .
I1 Cu1 P1 C7 -169.42(17) . .
I1 Cu1 P1 C7 -60.29(18) 2_665 .
Cu2 Cu1 P1 C7 -114.85(18) . .
N2 Cu1 P1 C1 -55.4(3) 7_575 .
I1 Cu1 P1 C1 71.71(18) . .
I1 Cu1 P1 C1 -179.16(17) 2_665 .
Cu2 Cu1 P1 C1 126.28(17) . .
N2 Cu1 P1 C13 -175.8(3) 7_575 .
I1 Cu1 P1 C13 -48.72(18) . .
I1 Cu1 P1 C13 60.41(17) 2_665 .
Cu2 Cu1 P1 C13 5.85(17) . .
I1 Cu2 N1 C19 -156.5(3) . 2_665
I1 Cu2 N1 C19 23.5(3) 2_665 2_665
Cu1 Cu2 N1 C19 113.7(3) . 2_665
Cu1 Cu2 N1 C19 -66.3(3) 2_665 2_665
I1 Cu2 N1 C19 23.5(3) . .
I1 Cu2 N1 C19 -156.5(3) 2_665 .
Cu1 Cu2 N1 C19 -66.3(3) . .
Cu1 Cu2 N1 C19 113.7(3) 2_665 .
C7 P1 C1 C2 14.5(4) . .
C13 P1 C1 C2 -94.3(4) . .
Cu1 P1 C1 C2 138.4(3) . .
C7 P1 C1 C6 -166.8(3) . .
C13 P1 C1 C6 84.4(3) . .
Cu1 P1 C1 C6 -42.8(3) . .
C6 C1 C2 C3 0.0 . .
P1 C1 C2 C3 178.7(4) . .
C1 C2 C3 C4 0.0 . .
C2 C3 C4 C5 0.0 . .
C3 C4 C5 C6 0.0 . .
C4 C5 C6 C1 0.0 . .
C2 C1 C6 C5 0.0 . .
P1 C1 C6 C5 -178.8(4) . .
C1 P1 C7 C8 -77.4(3) . .
C13 P1 C7 C8 32.4(3) . .
Cu1 P1 C7 C8 160.3(2) . .
C1 P1 C7 C12 101.3(3) . .
C13 P1 C7 C12 -148.9(3) . .
Cu1 P1 C7 C12 -21.0(3) . .
C12 C7 C8 C9 0.0 . .
P1 C7 C8 C9 178.7(4) . .
C7 C8 C9 C10 0.0 . .
C8 C9 C10 C11 0.0 . .
C9 C10 C11 C12 0.0 . .
C10 C11 C12 C7 0.0 . .
C8 C7 C12 C11 0.0 . .
P1 C7 C12 C11 -178.8(3) . .
C7 P1 C13 C14 -115.6(3) . .
C1 P1 C13 C14 -5.6(3) . .
Cu1 P1 C13 C14 118.3(2) . .
C7 P1 C13 C18 65.1(3) . .
C1 P1 C13 C18 175.2(3) . .
Cu1 P1 C13 C18 -61.0(3) . .
C18 C13 C14 C15 0.0 . .
P1 C13 C14 C15 -179.2(3) . .
C13 C14 C15 C16 0.0 . .
C14 C15 C16 C17 0.0 . .
C15 C16 C17 C18 0.0 . .
C16 C17 C18 C13 0.0 . .
C14 C13 C18 C17 0.0 . .
P1 C13 C18 C17 179.3(3) . .
N2 N2 C19 N1 -1.0(8) 2_665 .
Cu1 N2 C19 N1 179.8(4) 7_576 .
N2 N2 C19 C20 -179.4(7) 2_665 .
Cu1 N2 C19 C20 1.4(11) 7_576 .
C19 N1 C19 N2 0.4(3) 2_665 .
Cu2 N1 C19 N2 -179.6(3) . .
C19 N1 C19 C20 178.7(8) 2_665 .
Cu2 N1 C19 C20 -1.3(8) . .
