#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/24/8102484.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_8102484
loop_
_publ_author_name
'Zheng-Jing Jiang'
'Yu Zhang'
'Guo-Dong Tang'
'Jian-Ying Zhao'
'Lu-De Lu'
_publ_section_title
;
 Crystal structure of tetra-m3-iodo-tetrakis[(nicotine)copper(I)],
 Cu4I4(C10H14N2)4
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              466
_journal_volume                  224
_journal_year                    2009
_chemical_absolute_configuration trans
_chemical_formula_moiety         'C40 H56 Cu4 I4 N8'
_chemical_formula_sum            'C40 H56 Cu4 I4 N8'
_chemical_formula_weight         1410.69
_chemical_name_systematic
; 
tetrakis-μ₃-iodido-
tetrakis[(nicotine)copper(I)]
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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            2
_cell_length_a                   13.3880(2)
_cell_length_b                   14.7605(3)
_cell_length_c                   12.3126(2)
_cell_measurement_reflns_used    4625
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.13
_cell_volume                     2433.14(7)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXL97
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Aepex II CCD '
_diffrn_measurement_method       'phi and omega 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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13592
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    4.298
_exptl_absorpt_correction_T_max  0.548
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            LIGHT-YELLOW
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.363
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack (1983), 1909 Friedel pairs'
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+1.9900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                3903
_reflns_number_total             4625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2673.cff
_cod_data_source_block           1
_cod_database_code               8102484
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'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5181(7) 0.7048(6) 0.4913(9) 0.042(2) Uani 1 1 d . . .
H1 H 0.5837 0.6845 0.4963 0.051 Uiso 1 1 calc R . .
C2 C 0.4878(7) 0.7564(6) 0.4028(9) 0.040(2) Uani 1 1 d . . .
C3 C 0.3913(7) 0.7925(7) 0.3964(10) 0.049(3) Uani 1 1 d . . .
H3 H 0.3702 0.8276 0.3379 0.059 Uiso 1 1 calc R . .
C4 C 0.3289(9) 0.7721(7) 0.4839(8) 0.047(3) Uani 1 1 d . . .
H4 H 0.2650 0.7967 0.4844 0.057 Uiso 1 1 calc R . .
C5 C 0.3567(8) 0.7179(6) 0.5689(8) 0.039(2) Uani 1 1 d . . .
H5 H 0.3117 0.7043 0.6241 0.046 Uiso 1 1 calc R . .
C6 C 0.5690(7) 0.7762(6) 0.3134(7) 0.033(2) Uani 1 1 d . . .
H6 H 0.6316 0.7462 0.3337 0.040 Uiso 1 1 calc R . .
C7 C 0.5880(8) 0.8743(6) 0.2978(8) 0.044(3) Uani 1 1 d . . .
H7A H 0.6401 0.8958 0.3461 0.053 Uiso 1 1 calc R . .
H7B H 0.5279 0.9096 0.3095 0.053 Uiso 1 1 calc R . .
C8 C 0.6232(8) 0.8784(7) 0.1727(9) 0.047(3) Uani 1 1 d . . .
H8A H 0.5782 0.9144 0.1285 0.056 Uiso 1 1 calc R . .
H8B H 0.6908 0.9012 0.1653 0.056 Uiso 1 1 calc R . .
C9 C 0.6159(8) 0.7732(7) 0.1450(9) 0.047(3) Uani 1 1 d . . .
H9A H 0.6048 0.7647 0.0679 0.056 Uiso 1 1 calc R . .
H9B H 0.6774 0.7428 0.1650 0.056 Uiso 1 1 calc R . .
C10 C 0.5294(7) 0.6382(6) 0.2087(10) 0.049(3) Uani 1 1 d . . .
H10A H 0.5959 0.6156 0.2192 0.074 Uiso 1 1 calc R . .
H10B H 0.5037 0.6165 0.1407 0.074 Uiso 1 1 calc R . .
H10C H 0.4873 0.6175 0.2668 0.074 Uiso 1 1 calc R . .
C11 C 0.7143(8) 0.4927(7) 1.0462(8) 0.040(2) Uani 1 1 d . . .
H11 H 0.6607 0.4554 1.0638 0.047 Uiso 1 1 calc R . .
C12 C 0.7915(7) 0.4930(7) 1.1144(9) 0.045(3) Uani 1 1 d . . .
C13 C 0.8749(9) 0.5459(7) 1.0855(8) 0.049(3) Uani 1 1 d . . .
H13 H 0.9319 0.5466 1.1287 0.059 Uiso 1 1 calc R . .
C14 C 0.8702(7) 0.5965(7) 0.9923(8) 0.044(2) Uani 1 1 d . . .
H14 H 0.9233 0.6337 0.9725 0.053 Uiso 1 1 calc R . .
C15 C 0.7885(7) 0.5918(7) 0.9303(9) 0.041(2) Uani 1 1 d . . .
H15 H 0.7892 0.6257 0.8666 0.050 Uiso 1 1 calc R . .
C16 C 0.7904(8) 0.4274(7) 1.2140(8) 0.043(2) Uani 1 1 d . . .
H16 H 0.7249 0.3985 1.2211 0.052 Uiso 1 1 calc R . .
C17 C 0.8201(9) 0.4716(8) 1.3194(9) 0.054(3) Uani 1 1 d . . .
H17A H 0.8714 0.5169 1.3072 0.064 Uiso 1 1 calc R . .
H17B H 0.7629 0.5006 1.3531 0.064 Uiso 1 1 calc R . .
C18 C 0.8575(9) 0.3995(7) 1.3873(9) 0.051(3) Uani 1 1 d . . .
H18A H 0.8115 0.3879 1.4465 0.061 Uiso 1 1 calc R . .
H18B H 0.9217 0.4162 1.4179 0.061 Uiso 1 1 calc R . .
C19 C 0.8683(9) 0.3154(7) 1.3167(9) 0.051(3) Uani 1 1 d . . .
H19A H 0.9301 0.2833 1.3313 0.061 Uiso 1 1 calc R . .
H19B H 0.8123 0.2744 1.3253 0.061 Uiso 1 1 calc R . .
C20 C 0.8357(9) 0.2938(7) 1.1267(10) 0.057(3) Uani 1 1 d . . .
H20A H 0.8134 0.3256 1.0631 0.069 Uiso 1 1 calc R . .
H20C H 0.7817 0.2585 1.1557 0.069 Uiso 1 1 calc R . .
H20B H 0.8901 0.2545 1.1078 0.069 Uiso 1 1 calc R . .
Cu1 Cu 0.59273(8) 0.52489(7) 0.84553(9) 0.0314(3) Uani 1 1 d . . .
Cu2 Cu 0.48342(8) 0.58867(7) 0.68553(8) 0.0297(3) Uani 1 1 d . . .
I1 I 0.44932(4) 0.64986(4) 0.88287(4) 0.02980(15) Uani 1 1 d . . .
I2 I 0.66779(4) 0.53349(4) 0.64127(5) 0.03221(15) Uani 1 1 d . . .
N1 N 0.4507(6) 0.6842(5) 0.5710(6) 0.0336(18) Uani 1 1 d . . .
N2 N 0.5312(6) 0.7360(5) 0.2079(5) 0.040(2) Uani 1 1 d . . .
N3 N 0.7060(6) 0.5437(6) 0.9498(7) 0.045(2) Uani 1 1 d . . .
N4 N 0.8690(6) 0.3589(6) 1.2078(7) 0.0391(19) Uani 1 1 d . . .
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'
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
_geom_angle_publ_flag
N1 C1 C2 119.4(9) . . ?
N1 C1 H1 120.3 . . ?
C2 C1 H1 120.3 . . ?
C1 C2 C3 121.5(9) . . ?
C1 C2 C6 116.6(8) . . ?
C3 C2 C6 121.8(8) . . ?
C4 C3 C2 115.2(10) . . ?
C4 C3 H3 122.4 . . ?
C2 C3 H3 122.4 . . ?
C5 C4 C3 123.6(10) . . ?
C5 C4 H4 118.2 . . ?
C3 C4 H4 118.2 . . ?
N1 C5 C4 118.8(9) . . ?
N1 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C7 C6 N2 109.2(7) . . ?
C7 C6 C2 113.0(8) . . ?
N2 C6 C2 107.2(7) . . ?
C7 C6 H6 109.1 . . ?
N2 C6 H6 109.1 . . ?
C2 C6 H6 109.1 . . ?
C6 C7 C8 102.2(7) . . ?
C6 C7 H7A 111.3 . . ?
C8 C7 H7A 111.3 . . ?
C6 C7 H7B 111.3 . . ?
C8 C7 H7B 111.3 . . ?
H7A C7 H7B 109.2 . . ?
C9 C8 C7 98.6(7) . . ?
C9 C8 H8A 112.1 . . ?
C7 C8 H8A 112.1 . . ?
C9 C8 H8B 112.1 . . ?
C7 C8 H8B 112.1 . . ?
H8A C8 H8B 109.7 . . ?
N2 C9 C8 107.3(8) . . ?
N2 C9 H9A 110.3 . . ?
C8 C9 H9A 110.3 . . ?
N2 C9 H9B 110.3 . . ?
C8 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N3 126.2(10) . . ?
C12 C11 H11 116.9 . . ?
N3 C11 H11 116.9 . . ?
C11 C12 C13 117.2(10) . . ?
C11 C12 C16 119.1(9) . . ?
C13 C12 C16 123.3(9) . . ?
C14 C13 C12 118.6(10) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C15 C14 C13 119.2(10) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
N3 C15 C14 127.0(11) . . ?
N3 C15 H15 116.5 . . ?
C14 C15 H15 116.5 . . ?
N4 C16 C17 98.9(8) . . ?
N4 C16 C12 112.4(8) . . ?
C17 C16 C12 113.9(9) . . ?
N4 C16 H16 110.4 . . ?
C17 C16 H16 110.4 . . ?
C12 C16 H16 110.4 . . ?
C18 C17 C16 105.7(9) . . ?
C18 C17 H17A 110.6 . . ?
C16 C17 H17A 110.6 . . ?
C18 C17 H17B 110.6 . . ?
C16 C17 H17B 110.6 . . ?
H17A C17 H17B 108.7 . . ?
C17 C18 C19 107.7(9) . . ?
C17 C18 H18A 110.2 . . ?
C19 C18 H18A 110.2 . . ?
C17 C18 H18B 110.2 . . ?
C19 C18 H18B 110.2 . . ?
H18A C18 H18B 108.5 . . ?
N4 C19 C18 99.4(8) . . ?
N4 C19 H19A 111.9 . . ?
C18 C19 H19A 111.9 . . ?
N4 C19 H19B 111.9 . . ?
C18 C19 H19B 111.9 . . ?
H19A C19 H19B 109.6 . . ?
N4 C20 H20A 109.5 . . ?
N4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
N4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20C C20 H20B 109.5 . . ?
N3 Cu1 Cu1 139.8(2) . 2_665 ?
N3 Cu1 Cu2 148.3(3) . . ?
Cu1 Cu1 Cu2 64.39(4) 2_665 . ?
N3 Cu1 I1 100.5(3) . 2_665 ?
Cu1 Cu1 I1 61.67(4) 2_665 2_665 ?
Cu2 Cu1 I1 110.87(5) . 2_665 ?
N3 Cu1 I1 109.5(2) . . ?
Cu1 Cu1 I1 60.81(4) 2_665 . ?
Cu2 Cu1 I1 59.16(3) . . ?
I1 Cu1 I1 118.59(4) 2_665 . ?
N3 Cu1 I2 107.9(2) . . ?
Cu1 Cu1 I2 111.63(3) 2_665 . ?
Cu2 Cu1 I2 59.62(3) . . ?
I1 Cu1 I2 106.39(4) 2_665 . ?
I1 Cu1 I2 112.91(4) . . ?
N3 Cu1 Cu2 144.5(2) . 2_665 ?
Cu1 Cu1 Cu2 58.49(4) 2_665 2_665 ?
Cu2 Cu1 Cu2 58.71(5) . 2_665 ?
I1 Cu1 Cu2 57.61(3) 2_665 2_665 ?
I1 Cu1 Cu2 105.76(4) . 2_665 ?
I2 Cu1 Cu2 60.45(3) . 2_665 ?
N1 Cu2 Cu1 152.2(2) . . ?
N1 Cu2 I1 111.3(2) . . ?
Cu1 Cu2 I1 61.81(3) . . ?
N1 Cu2 Cu2 135.8(2) . 2_665 ?
Cu1 Cu2 Cu2 63.50(4) . 2_665 ?
I1 Cu2 Cu2 111.55(3) . 2_665 ?
N1 Cu2 I2 105.6(2) . . ?
Cu1 Cu2 I2 61.74(4) . . ?
I1 Cu2 I2 117.12(4) . . ?
Cu2 Cu2 I2 62.76(4) 2_665 . ?
N1 Cu2 I2 99.1(2) . 2_665 ?
Cu1 Cu2 I2 108.77(4) . 2_665 ?
I1 Cu2 I2 106.18(4) . 2_665 ?
Cu2 Cu2 I2 58.64(4) 2_665 2_665 ?
I2 Cu2 I2 116.11(4) . 2_665 ?
N1 Cu2 Cu1 145.8(2) . 2_665 ?
Cu1 Cu2 Cu1 57.12(5) . 2_665 ?
I1 Cu2 Cu1 59.28(3) . 2_665 ?
Cu2 Cu2 Cu1 57.79(4) 2_665 2_665 ?
I2 Cu2 Cu1 107.54(4) . 2_665 ?
I2 Cu2 Cu1 58.54(3) 2_665 2_665 ?
Cu2 I1 Cu1 63.11(4) . 2_665 ?
Cu2 I1 Cu1 59.03(3) . . ?
Cu1 I1 Cu1 57.52(4) 2_665 . ?
Cu2 I2 Cu1 58.64(3) . . ?
Cu2 I2 Cu2 58.61(4) . 2_665 ?
Cu1 I2 Cu2 61.01(3) . 2_665 ?
C5 N1 C1 121.3(8) . . ?
C5 N1 Cu2 117.7(6) . . ?
C1 N1 Cu2 120.5(6) . . ?
C10 N2 C9 112.8(8) . . ?
C10 N2 C6 113.0(7) . . ?
C9 N2 C6 92.7(8) . . ?
C15 N3 C11 111.8(9) . . ?
C15 N3 Cu1 125.7(8) . . ?
C11 N3 Cu1 121.6(7) . . ?
C20 N4 C16 105.8(8) . . ?
C20 N4 C19 109.3(8) . . ?
C16 N4 C19 104.3(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.367(12) . ?
C1 C2 1.390(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.399(13) . ?
C2 C6 1.575(12) . ?
C3 C4 1.396(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.369(13) . ?
C4 H4 0.9300 . ?
C5 N1 1.354(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.482(13) . ?
C6 N2 1.515(12) . ?
C6 H6 0.9800 . ?
C7 C8 1.612(13) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.592(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.478(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.444(12) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.332(13) . ?
C11 N3 1.409(14) . ?
C11 H11 0.9300 . ?
C12 C13 1.409(14) . ?
C12 C16 1.563(14) . ?
C13 C14 1.369(15) . ?
C13 H13 0.9300 . ?
C14 C15 1.336(14) . ?
C14 H14 0.9300 . ?
C15 N3 1.335(12) . ?
C15 H15 0.9300 . ?
C16 N4 1.461(12) . ?
C16 C17 1.505(15) . ?
C16 H16 0.9800 . ?
C17 C18 1.443(15) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.523(13) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N4 1.486(14) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N4 1.456(13) . ?
C20 H20A 0.9600 . ?
C20 H20C 0.9600 . ?
C20 H20B 0.9600 . ?
Cu1 N3 2.007(9) . ?
Cu1 Cu1 2.589(2) 2_665 ?
Cu1 Cu2 2.6285(14) . ?
Cu1 I1 2.6798(12) 2_665 ?
Cu1 I1 2.7018(12) . ?
Cu1 I2 2.7113(12) . ?
Cu1 Cu2 2.7803(15) 2_665 ?
Cu2 N1 2.042(7) . ?
Cu2 I1 2.6322(12) . ?
Cu2 Cu2 2.655(2) 2_665 ?
Cu2 I2 2.6557(12) . ?
Cu2 I2 2.7652(13) 2_665 ?
Cu2 Cu1 2.7803(15) 2_665 ?
I1 Cu1 2.6798(12) 2_665 ?
I2 Cu2 2.7652(13) 2_665 ?
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
C19 H19A N1 0.97 2.48 3.395(14) 158.1 3_647
C20 H20B I1 0.96 2.65 3.579(11) 163.2 3_647
