#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:26:50 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179896 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/92/7019254.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_7019254
loop_
_publ_author_name
'Scepaniak, Jeremiah J.'
'Wu, Guang'
'Hayton, Trevor W.'
_publ_section_title
;
 Complexes of Cu(i) supported by a tris(ketimine) tripod.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7859
_journal_page_last               7861
_journal_paper_doi               10.1039/c2dt30101f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C92 H81 Cu3 I3 N15'
_chemical_formula_weight         1968.04
_chemical_name_common            '[N(ArCNHPh)3Cu]2[CuI3]'
_chemical_name_systematic
;
?
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.9356(8)
_cell_length_b                   16.9356(8)
_cell_length_c                   17.9643(8)
_cell_measurement_temperature    100(2)
_cell_volume                     4462.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       'omega scan'
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26538
_diffrn_reflns_theta_full        35.19
_diffrn_reflns_theta_max         35.19
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.799
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         6797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0495P)²+1.8043P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                4969
_reflns_number_total             6797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30101f.txt
_cod_data_source_block           compound_3
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               7019254
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
C1 C 0.75488(12) 0.24059(12) 0.48018(9) 0.0161(3) Uani 1 1 d .
C2 C 0.83337(12) 0.22476(11) 0.48862(10) 0.0172(3) Uani 1 1 d .
C3 C 0.88253(13) 0.22389(13) 0.42621(11) 0.0218(3) Uani 1 1 d .
H3 H 0.8640 0.2304 0.3778 0.026 Uiso 1 1 calc R
C4 C 0.95856(13) 0.21340(14) 0.43514(12) 0.0260(4) Uani 1 1 d .
H4 H 0.9912 0.2119 0.3927 0.031 Uiso 1 1 calc R
C5 C 0.98669(13) 0.20516(13) 0.50574(13) 0.0265(4) Uani 1 1 d .
H5 H 1.0390 0.1988 0.5115 0.032 Uiso 1 1 calc R
C6 C 0.93854(14) 0.20621(14) 0.56818(12) 0.0255(4) Uani 1 1 d .
H6 H 0.9581 0.2012 0.6166 0.031 Uiso 1 1 calc R
C7 C 0.86147(13) 0.21466(13) 0.55911(10) 0.0210(3) Uani 1 1 d .
H7 H 0.8275 0.2135 0.6016 0.025 Uiso 1 1 calc R
C8 C 0.67774(12) 0.19508(11) 0.53418(9) 0.0157(3) Uani 1 1 d .
C9 C 0.63753(11) 0.23886(11) 0.57277(9) 0.0144(3) Uani 1 1 d .
C10 C 0.56655(13) 0.18852(13) 0.62279(10) 0.0195(3) Uani 1 1 d .
H10 H 0.5421 0.2185 0.6514 0.023 Uiso 1 1 calc R
C11 C 0.53108(13) 0.09489(14) 0.63130(11) 0.0238(4) Uani 1 1 d .
H11 H 0.4820 0.0614 0.6647 0.029 Uiso 1 1 calc R
C12 C 0.56737(14) 0.05066(14) 0.59105(12) 0.0257(4) Uani 1 1 d .
H12 H 0.5419 -0.0135 0.5952 0.031 Uiso 1 1 calc R
C13 C 0.64164(13) 0.10152(12) 0.54451(11) 0.0209(3) Uani 1 1 d .
H13 H 0.6685 0.0717 0.5190 0.025 Uiso 1 1 calc R
C14 C 0.0000 0.0000 0.593(4) 0.24(8) Uani 0.50 3 d SP
C15 C 0.0000 0.0000 0.670(5) 0.27(7) Uani 0.50 3 d SP
H15A H -0.0356 0.0272 0.6883 0.401 Uiso 0.17 1 calc PR
H15B H 0.0628 0.0356 0.6883 0.401 Uiso 0.17 1 calc PR
H15C H -0.0272 -0.0628 0.6883 0.401 Uiso 0.17 1 calc PR
C16 C 0.0980(4) 0.2846(3) 0.7500 0.0582(12) Uani 1 2 d S
C17 C 0.0883(4) 0.3609(4) 0.7500 0.0792(17) Uani 1 2 d S
H17A H 0.0271 0.3442 0.7327 0.119 Uiso 0.50 1 calc PR
H17B H 0.1339 0.4071 0.7167 0.119 Uiso 0.50 1 calc PR
H17C H 0.0973 0.3856 0.8006 0.119 Uiso 0.50 1 calc PR
C18 C 0.3760(3) 0.2223(4) 0.7500 0.0526(11) Uani 1 2 d S
C19 C 0.3523(4) 0.2931(3) 0.7500 0.0560(11) Uani 1 2 d S
H19A H 0.3567 0.3161 0.8008 0.084 Uiso 0.50 1 calc PR
H19B H 0.2897 0.2682 0.7318 0.084 Uiso 0.50 1 calc PR
H19C H 0.3942 0.3430 0.7175 0.084 Uiso 0.50 1 calc PR
Cu2 Cu 0.6667 0.3333 0.41249(2) 0.01664(8) Uani 1 3 d S
Cu3 Cu 0.6667 0.3333 0.2500 0.02429(13) Uani 1 6 d S
I1 I 0.545148(14) 0.161674(13) 0.2500 0.02627(6) Uani 1 2 d S
N1 N 0.75080(10) 0.28912(10) 0.42708(8) 0.0184(3) Uani 1 1 d .
H1 H 0.7925 0.3045 0.3922 0.022 Uiso 1 1 calc R
N2 N 0.6667 0.3333 0.56250(13) 0.0145(4) Uani 1 3 d S
N3 N 0.0000 0.0000 0.5000 0.19(2) Uani 1 6 d S
N4 N 0.1095(5) 0.2251(4) 0.7500 0.104(2) Uani 1 2 d S
N5 N 0.3945(4) 0.1652(5) 0.7500 0.0875(18) Uani 1 2 d S
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
N1 C1 C2 121.99(15) . .
N1 C1 C8 119.96(16) . .
C2 C1 C8 118.02(15) . .
C7 C2 C3 119.00(17) . .
C7 C2 C1 120.33(15) . .
C3 C2 C1 120.60(16) . .
C4 C3 C2 120.05(19) . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C5 C4 C3 120.26(19) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 120.19(18) . .
C4 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C5 C6 C7 119.50(19) . .
C5 C6 H6 120.2 . .
C7 C6 H6 120.2 . .
C6 C7 C2 120.96(18) . .
C6 C7 H7 119.5 . .
C2 C7 H7 119.5 . .
C13 C8 C9 118.52(16) . .
C13 C8 C1 116.43(15) . .
C9 C8 C1 125.01(15) . .
C10 C9 C8 119.21(15) . .
C10 C9 N2 118.39(15) . .
C8 C9 N2 122.40(15) . .
C11 C10 C9 120.92(17) . .
C11 C10 H10 119.5 . .
C9 C10 H10 119.5 . .
C12 C11 C10 120.12(17) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C11 C12 C13 119.10(18) . .
C11 C12 H12 120.5 . .
C13 C12 H12 120.5 . .
C12 C13 C8 121.94(17) . .
C12 C13 H13 119.0 . .
C8 C13 H13 119.0 . .
C15 C14 N3 180.000(15) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N4 C16 C17 177.2(7) . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
N5 C18 C19 179.6(6) . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
N1 Cu2 N1 118.19(2) . 3_665
N1 Cu2 N1 118.19(2) . 2_655
N1 Cu2 N1 118.19(2) 3_665 2_655
N1 Cu2 N1 118.19(2) . 2_655
N1 Cu2 N1 118.19(2) 3_665 2_655
N1 Cu2 N1 0.00(13) 2_655 2_655
N1 Cu2 Cu3 97.80(5) . .
N1 Cu2 Cu3 97.80(5) 3_665 .
N1 Cu2 Cu3 97.80(5) 2_655 .
N1 Cu2 Cu3 97.80(5) 2_655 .
I1 Cu3 I1 120.0 2_655 3_665
I1 Cu3 I1 120.0 2_655 .
I1 Cu3 I1 120.0 3_665 .
I1 Cu3 Cu2 90.0 2_655 .
I1 Cu3 Cu2 90.0 3_665 .
I1 Cu3 Cu2 90.0 . .
I1 Cu3 Cu2 90.0 2_655 10_556
I1 Cu3 Cu2 90.0 3_665 10_556
I1 Cu3 Cu2 90.0 . 10_556
Cu2 Cu3 Cu2 180.0 . 10_556
C1 N1 Cu2 129.49(13) . .
C1 N1 H1 115.3 . .
Cu2 N1 H1 115.3 . .
C9 N2 C9 118.36(5) . 2_655
C9 N2 C9 118.36(5) . 3_665
C9 N2 C9 118.36(5) 2_655 3_665
C14 N3 C14 180.000(8) . 7_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.283(2) .
C1 C2 1.489(2) .
C1 C8 1.495(2) .
C2 C7 1.393(3) .
C2 C3 1.401(2) .
C3 C4 1.394(3) .
C3 H3 0.9500 .
C4 C5 1.386(3) .
C4 H4 0.9500 .
C5 C6 1.392(3) .
C5 H5 0.9500 .
C6 C7 1.392(3) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 C13 1.397(2) .
C8 C9 1.414(2) .
C9 C10 1.398(2) .
C9 N2 1.4310(16) .
C10 C11 1.395(3) .
C10 H10 0.9500 .
C11 C12 1.386(3) .
C11 H11 0.9500 .
C12 C13 1.393(3) .
C12 H12 0.9500 .
C13 H13 0.9500 .
C14 C15 1.38(14) .
C14 N3 1.67(8) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 N4 1.118(7) .
C16 C17 1.382(8) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 N5 1.155(6) .
C18 C19 1.443(7) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
Cu2 N1 1.9304(16) .
Cu2 N1 1.9304(16) 3_665
Cu2 N1 1.9304(16) 2_655
Cu2 N1 1.9304(16) 2_655
Cu2 Cu3 2.9190(4) .
Cu3 I1 2.5892(2) 2_655
Cu3 I1 2.5892(2) 3_665
Cu3 I1 2.5892(2) .
Cu3 Cu2 2.9190(4) 10_556
N1 H1 0.8800 .
N2 C9 1.4310(17) 2_655
N2 C9 1.4310(16) 3_665
N3 C14 1.67(8) 7_556
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
N1 C1 C2 C7 147.56(18) . .
C8 C1 C2 C7 -34.7(2) . .
N1 C1 C2 C3 -29.5(3) . .
C8 C1 C2 C3 148.16(17) . .
C7 C2 C3 C4 -0.3(3) . .
C1 C2 C3 C4 176.90(17) . .
C2 C3 C4 C5 -1.0(3) . .
C3 C4 C5 C6 0.8(3) . .
C4 C5 C6 C7 0.7(3) . .
C5 C6 C7 C2 -1.9(3) . .
C3 C2 C7 C6 1.7(3) . .
C1 C2 C7 C6 -175.47(17) . .
N1 C1 C8 C13 127.28(19) . .
C2 C1 C8 C13 -50.5(2) . .
N1 C1 C8 C9 -50.4(2) . .
C2 C1 C8 C9 131.84(18) . .
C13 C8 C9 C10 3.4(3) . .
C1 C8 C9 C10 -178.96(16) . .
C13 C8 C9 N2 -176.48(17) . .
C1 C8 C9 N2 1.2(3) . .
C8 C9 C10 C11 -4.3(3) . .
N2 C9 C10 C11 175.57(17) . .
C9 C10 C11 C12 1.3(3) . .
C10 C11 C12 C13 2.5(3) . .
C11 C12 C13 C8 -3.4(3) . .
C9 C8 C13 C12 0.4(3) . .
C1 C8 C13 C12 -177.43(18) . .
N1 Cu2 Cu3 I1 -36.32(5) . 2_655
N1 Cu2 Cu3 I1 -156.32(5) 3_665 2_655
N1 Cu2 Cu3 I1 83.68(5) 2_655 2_655
N1 Cu2 Cu3 I1 83.68(5) 2_655 2_655
N1 Cu2 Cu3 I1 -156.32(5) . 3_665
N1 Cu2 Cu3 I1 83.68(5) 3_665 3_665
N1 Cu2 Cu3 I1 -36.32(5) 2_655 3_665
N1 Cu2 Cu3 I1 -36.32(5) 2_655 3_665
N1 Cu2 Cu3 I1 83.68(5) . .
N1 Cu2 Cu3 I1 -36.32(5) 3_665 .
N1 Cu2 Cu3 I1 -156.32(5) 2_655 .
N1 Cu2 Cu3 I1 -156.32(5) 2_655 .
N1 Cu2 Cu3 Cu2 -170(5) . 10_556
N1 Cu2 Cu3 Cu2 70(5) 3_665 10_556
N1 Cu2 Cu3 Cu2 -50(5) 2_655 10_556
N1 Cu2 Cu3 Cu2 -50(5) 2_655 10_556
C2 C1 N1 Cu2 -170.23(12) . .
C8 C1 N1 Cu2 12.1(3) . .
N1 Cu2 N1 C1 -46.0(2) 3_665 .
N1 Cu2 N1 C1 107.54(14) 2_655 .
N1 Cu2 N1 C1 107.54(14) 2_655 .
Cu3 Cu2 N1 C1 -149.23(16) . .
C10 C9 N2 C9 125.61(16) . 2_655
C8 C9 N2 C9 -54.5(3) . 2_655
C10 C9 N2 C9 -29.2(3) . 3_665
C8 C9 N2 C9 150.67(17) . 3_665
C15 C14 N3 C14 0.0 . 7_556
