#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:07:32 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179524 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/21/4342190.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_4342190
loop_
_publ_author_name
'Reger, Daniel L.'
'Pascui, Andrea E.'
'Smith, Mark D.'
'Jezierska, Julia'
'Ozarowski, Andrew'
_publ_section_title
;
 Syntheses, Structural, Magnetic, and Electron Paramagnetic Resonance
 Studies of Monobridged Cyanide and Azide Dinuclear Copper(II) Complexes:
 Antiferromagnetic Superexchange Interactions.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1487
_journal_page_last               1500
_journal_paper_doi               10.1021/ic502485p
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C56 H68 Cu5 I4 N16, I3'
_chemical_formula_sum            'C56 H68 Cu5 I7 N16'
_chemical_formula_weight         2171.66
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_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
_audit_creation_date             2012-05-08
_audit_creation_method
;
  Olex2 1.2
  (compiled May  4 2012 14:03:18, GUI svn.r4222)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.768(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.632(2)
_cell_length_b                   21.904(3)
_cell_length_c                   8.5445(10)
_cell_measurement_reflns_used    7109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.40
_cell_volume                     3648.7(8)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26709
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.86
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           38.0
_diffrn_source_power             1.786
_diffrn_source_target            Mo
_diffrn_source_voltage           47.0
_exptl_absorpt_coefficient_mu    4.442
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.758136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0591 before and 0.0432 after correction.
The Ratio of minimum to maximum transmission is 0.7581.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.749
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0427
_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)+(0.0548P)²+18.3475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                3349
_reflns_number_total             3854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502485p_si_001.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4342186--4342190.cif.'
_cod_original_cell_volume        3648.8(7)
_cod_database_code               4342190
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z'
5 '-x, -y, -z'
6 'x, -y, z'
7 '-x+1/2, -y+1/2, -z'
8 '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
Cu1 Cu 0.38566(3) 0.60460(3) 0.45287(8) 0.02372(18) Uani 1 1 d .
Cu2 Cu 0.5000 0.54765(8) 0.5000 0.0179(4) Uani 0.50 2 d SP
I1 I 0.40624(2) 0.5000 0.31203(5) 0.01682(14) Uani 1 2 d S
I2 I 0.5000 0.66805(2) 0.5000 0.02552(15) Uani 1 2 d S
N11 N 0.3112(2) 0.6546(2) 0.3227(5) 0.0255(10) Uani 1 1 d .
N12 N 0.2504(2) 0.6634(2) 0.3829(5) 0.0249(10) Uani 1 1 d .
N21 N 0.3331(2) 0.6001(2) 0.6449(5) 0.0236(10) Uani 1 1 d .
N22 N 0.2638(2) 0.6105(2) 0.6320(5) 0.0206(9) Uani 1 1 d .
C1 C 0.2239(3) 0.6156(3) 0.4779(6) 0.0251(12) Uani 1 1 d .
H1 H 0.1765 0.6282 0.4965 0.030 Uiso 1 1 calc R
C2 C 0.2172(3) 0.5553(3) 0.3915(6) 0.0260(12) Uani 1 1 d .
C3 C 0.1948(3) 0.5545(3) 0.2291(6) 0.0316(14) Uani 1 1 d .
H3 H 0.1870 0.5919 0.1734 0.038 Uiso 1 1 calc R
C4 C 0.1841(5) 0.5000 0.1506(10) 0.039(2) Uani 1 2 d S
H4 H 0.1692 0.5000 0.0407 0.046 Uiso 1 2 calc SR
C5 C 0.2281(4) 0.5000 0.4705(9) 0.0238(16) Uani 1 2 d S
H5 H 0.2432 0.5000 0.5803 0.029 Uiso 1 2 calc SR
C11 C 0.2159(3) 0.7136(3) 0.3190(6) 0.0297(13) Uani 1 1 d .
C12 C 0.2572(3) 0.7387(3) 0.2164(7) 0.0330(14) Uani 1 1 d .
H12 H 0.2481 0.7744 0.1540 0.040 Uiso 1 1 calc R
C13 C 0.3157(3) 0.7010(3) 0.2222(6) 0.0294(13) Uani 1 1 d .
C14 C 0.1476(3) 0.7331(3) 0.3620(8) 0.0399(16) Uani 1 1 d .
H14A H 0.1136 0.7012 0.3312 0.060 Uiso 1 1 calc R
H14B H 0.1336 0.7712 0.3070 0.060 Uiso 1 1 calc R
H14C H 0.1508 0.7397 0.4761 0.060 Uiso 1 1 calc R
C15 C 0.3783(3) 0.7096(3) 0.1387(7) 0.0352(14) Uani 1 1 d .
H15A H 0.4089 0.7396 0.1960 0.053 Uiso 1 1 calc R
H15B H 0.3645 0.7244 0.0313 0.053 Uiso 1 1 calc R
H15C H 0.4024 0.6706 0.1342 0.053 Uiso 1 1 calc R
C21 C 0.2391(3) 0.6047(3) 0.7733(6) 0.0265(12) Uani 1 1 d .
C22 C 0.2949(3) 0.5924(3) 0.8815(7) 0.0280(13) Uani 1 1 d .
H22 H 0.2949 0.5861 0.9916 0.034 Uiso 1 1 calc R
C23 C 0.3519(3) 0.5909(2) 0.7968(6) 0.0228(11) Uani 1 1 d .
C24 C 0.1640(3) 0.6107(3) 0.7905(7) 0.0387(16) Uani 1 1 d .
H24A H 0.1465 0.6490 0.7423 0.058 Uiso 1 1 calc R
H24B H 0.1577 0.6106 0.9026 0.058 Uiso 1 1 calc R
H24C H 0.1390 0.5763 0.7378 0.058 Uiso 1 1 calc R
C25 C 0.4258(3) 0.5822(3) 0.8593(7) 0.0302(13) Uani 1 1 d .
H25A H 0.4484 0.5573 0.7854 0.045 Uiso 1 1 calc R
H25B H 0.4289 0.5617 0.9618 0.045 Uiso 1 1 calc R
H25C H 0.4484 0.6221 0.8717 0.045 Uiso 1 1 calc R
I3 I 0.0000 0.5000 0.5000 0.0459(4) Uani 0.840(3) 4 d SP
I4 I 0.0074(2) 0.63268(5) 0.4751(5) 0.0507(8) Uani 0.4198(14) 1 d P
I5 I 0.0000 0.5829(14) 0.0000 0.070 Uiso 0.043(2) 2 d SP
I6 I 0.0000 0.657(2) 0.0000 0.070 Uiso 0.041(3) 2 d SP
I7 I 0.0130(9) 0.6283(12) 0.042(2) 0.070 Uiso 0.039(2) 1 d P
I8 I 0.0000 0.4571(16) 0.0000 0.070 Uiso 0.037(2) 2 d SP
I9 I -0.001(2) 0.5000 0.033(4) 0.070 Uiso 0.027(2) 2 d SP
I10 I 0.0000 0.697(4) 0.0000 0.070 Uiso 0.016(2) 2 d SP
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'
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'
N N 0.0061 0.0033 '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 Cu1 I1 58.01(3) . .
Cu2 Cu1 I2 61.08(4) . .
I2 Cu1 I1 110.76(3) . .
N11 Cu1 Cu2 154.64(13) . .
N11 Cu1 I1 110.76(14) . .
N11 Cu1 I2 110.02(14) . .
N21 Cu1 Cu2 111.56(13) . .
N21 Cu1 I1 116.31(13) . .
N21 Cu1 I2 113.95(14) . .
N21 Cu1 N11 93.78(18) . .
Cu1 Cu2 Cu1 121.63(8) . 2_656
Cu1 Cu2 I2 60.81(4) . .
Cu1 Cu2 I2 60.81(4) 2_656 .
Cu2 Cu2 Cu1 119.19(4) 5_666 .
Cu2 Cu2 Cu1 119.19(4) 5_666 2_656
Cu2 Cu2 I1 65.55(4) 5_666 .
Cu2 Cu2 I1 65.56(4) 5_666 5_666
Cu2 Cu2 I2 179.999(1) 5_666 .
I1 Cu2 Cu1 62.647(18) 5_666 2_656
I1 Cu2 Cu1 149.67(2) 5_666 .
I1 Cu2 Cu1 149.67(2) . 2_656
I1 Cu2 Cu1 62.646(19) . .
I1 Cu2 I1 131.11(7) 5_666 .
I1 Cu2 I2 114.45(4) . .
I1 Cu2 I2 114.45(4) 5_666 .
Cu1 I1 Cu1 120.34(3) 6_565 .
Cu2 I1 Cu1 59.34(3) 5_666 6_565
Cu2 I1 Cu1 102.01(4) . 6_565
Cu2 I1 Cu1 59.35(3) . .
Cu2 I1 Cu1 102.02(4) 5_666 .
Cu2 I1 Cu2 48.89(7) 5_666 .
Cu1 I2 Cu1 116.21(3) 2_656 .
Cu1 I2 Cu2 58.103(17) 2_656 .
Cu1 I2 Cu2 58.102(17) . .
N12 N11 Cu1 118.0(3) . .
C13 N11 Cu1 131.1(4) . .
C13 N11 N12 105.1(4) . .
N11 N12 C1 119.5(4) . .
N11 N12 C11 112.0(5) . .
C11 N12 C1 127.4(5) . .
N22 N21 Cu1 121.2(3) . .
C23 N21 Cu1 133.4(4) . .
C23 N21 N22 105.3(4) . .
N21 N22 C1 120.6(4) . .
C21 N22 N21 111.6(4) . .
C21 N22 C1 126.9(5) . .
N12 C1 H1 106.8 . .
N12 C1 C2 111.8(4) . .
N22 C1 N12 111.7(5) . .
N22 C1 H1 106.8 . .
N22 C1 C2 112.4(5) . .
C2 C1 H1 106.8 . .
C3 C2 C1 119.5(5) . .
C5 C2 C1 121.7(5) . .
C5 C2 C3 118.7(6) . .
C2 C3 H3 119.8 . .
C4 C3 C2 120.3(6) . .
C4 C3 H3 119.8 . .
C3 C4 C3 120.7(8) 6_565 .
C3 C4 H4 119.6 . .
C3 C4 H4 119.6 6_565 .
C2 C5 C2 121.2(7) . 6_565
C2 C5 H5 119.4 . .
C2 C5 H5 119.4 6_565 .
N12 C11 C12 106.0(5) . .
N12 C11 C14 123.1(6) . .
C12 C11 C14 130.9(6) . .
C11 C12 H12 126.8 . .
C11 C12 C13 106.3(5) . .
C13 C12 H12 126.8 . .
N11 C13 C12 110.6(5) . .
N11 C13 C15 121.2(5) . .
C12 C13 C15 128.1(6) . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15B 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N22 C21 C22 106.0(5) . .
N22 C21 C24 122.4(5) . .
C22 C21 C24 131.6(5) . .
C21 C22 H22 126.9 . .
C21 C22 C23 106.2(5) . .
C23 C22 H22 126.9 . .
N21 C23 C22 110.8(5) . .
N21 C23 C25 121.1(5) . .
C22 C23 C25 128.1(5) . .
C21 C24 H24A 109.5 . .
C21 C24 H24B 109.5 . .
C21 C24 H24C 109.5 . .
H24A C24 H24B 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C23 C25 H25A 109.5 . .
C23 C25 H25B 109.5 . .
C23 C25 H25C 109.5 . .
H25A C25 H25B 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
I4 I3 I4 180.0 . 5_566
I4 I3 I4 169.31(9) 2_556 5_566
I4 I3 I4 169.31(9) . 6_565
I4 I3 I4 180.0 2_556 6_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu2 2.5581(11) .
Cu1 I1 2.6411(7) .
Cu1 I2 2.6305(8) .
Cu1 N11 2.047(5) .
Cu1 N21 2.041(4) .
Cu2 Cu1 2.5581(11) 2_656
Cu2 Cu2 2.087(4) 5_666
Cu2 I1 2.5219(9) .
Cu2 I1 2.5219(9) 5_666
Cu2 I2 2.6374(19) .
I1 Cu1 2.6410(7) 6_565
I1 Cu2 2.5219(9) 5_666
I2 Cu1 2.6305(8) 2_656
N11 N12 1.368(6) .
N11 C13 1.340(7) .
N12 C1 1.458(7) .
N12 C11 1.370(7) .
N21 N22 1.370(6) .
N21 C23 1.323(7) .
N22 C1 1.455(7) .
N22 C21 1.359(7) .
C1 H1 1.0000 .
C1 C2 1.511(8) .
C2 C3 1.406(8) .
C2 C5 1.391(7) .
C3 H3 0.9500 .
C3 C4 1.374(8) .
C4 C3 1.374(8) 6_565
C4 H4 0.9500 .
C5 C2 1.391(7) 6_565
C5 H5 0.9500 .
C11 C12 1.376(9) .
C11 C14 1.495(8) .
C12 H12 0.9500 .
C12 C13 1.411(8) .
C13 C15 1.504(8) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C21 C22 1.375(8) .
C21 C24 1.504(8) .
C22 H22 0.9500 .
C22 C23 1.403(7) .
C23 C25 1.497(8) .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
I3 I4 2.9189(12) 2_556
I3 I4 2.9190(12) .
I3 I4 2.9190(12) 5_566
I3 I4 2.9190(12) 6_565
I4 I4 0.544(4) 2_556
I5 I6 1.63(5) .
I5 I7 1.08(3) .
I5 I7 1.08(3) 2
I5 I8 0.88(3) 5_565
I5 I8 2.76(6) .
I5 I9 1.84(3) 5_565
I5 I9 1.84(3) .
I5 I10 2.51(8) .
I6 I7 0.76(3) 2
I6 I7 0.76(3) .
I6 I8 2.50(6) 5_565
I6 I10 0.88(6) .
I7 I7 0.83(4) 2
I7 I8 1.92(4) 5_565
I7 I9 2.82(3) .
I7 I9 2.89(3) 5_565
I7 I10 1.57(7) .
I8 I5 0.88(3) 5_565
I8 I6 2.50(6) 5_565
I8 I7 1.92(4) 5_565
I8 I7 1.92(4) 6_565
I8 I8 1.88(7) 5_565
I8 I9 0.98(3) 5_565
I8 I9 0.98(3) .
I9 I5 1.84(3) 5_565
I9 I7 2.82(3) 6_565
I9 I7 2.89(3) 5_565
I9 I7 2.89(3) 2
I9 I8 0.98(3) 5_565
I9 I9 0.57(7) 5_565
I10 I7 1.57(7) 2
