#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:49:05 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179457 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/54/4335432.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_4335432
loop_
_publ_author_name
'Sang Ho Lim'
'Seth M. Cohen'
_publ_section_title
;
 Self-Assembled Supramolecular Clusters Based on Phosphines and Coinage
 Metals: Tetrahedra, Helicates, and Mesocates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7862
_journal_page_last               7872
_journal_paper_doi               10.1021/ic302840x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '2(C99 H69 Cu2 I2 N3 P6), 3(C H2 Cl2)'
_chemical_formula_sum            'C201 H144 Cl6 Cu4 I4 N6 P12'
_chemical_formula_weight         3989.32
_chemical_name_common            '[Cu2(2,6-dppeb)3]I2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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            1
_cell_length_a                   13.1976(3)
_cell_length_b                   13.1976(3)
_cell_length_c                   38.5008(8)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.18
_cell_measurement_theta_min      3.86
_cell_volume                     5807.5(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            3433
_diffrn_reflns_theta_full        66.44
_diffrn_reflns_theta_max         66.44
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    6.335
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       plate
_exptl_crystal_F_000             2002
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.819
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.026(15)
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         3433
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0837
_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)+(0.1592P)²+16.9704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2424
_refine_ls_wR_factor_ref         0.2456
_reflns_number_gt                3271
_reflns_number_total             3433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302840x_si_002_07.cif
_cod_data_source_block           '[Cu2[2,6-dppeb]3]I2'
_cod_original_sg_symbol_H-M      'P -6 2 c '
_cod_database_code               4335432
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'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+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
_atom_site_disorder_group
I1 I 0.3333 0.6667 0.525762(18) 0.0646(4) Uani 1 3 d S .
Cu1 Cu 0.3333 0.6667 0.59260(4) 0.0384(4) Uani 1 3 d S .
P1 P 0.31075(16) 0.49625(16) 0.61451(4) 0.0382(4) Uani 1 1 d . .
N1 N 0.3994(8) 0.5464(8) 0.7500 0.049(2) Uani 1 2 d S .
C15 C 0.4617(6) 0.5790(6) 0.71865(15) 0.0408(16) Uani 1 1 d . .
C14 C 0.4043(7) 0.5441(7) 0.68552(17) 0.0484(19) Uani 1 1 d . .
C13 C 0.3635(7) 0.5156(7) 0.65745(18) 0.0464(17) Uani 1 1 d . .
C17 C 0.6418(10) 0.6811(12) 0.7500 0.051(3) Uani 1 2 d S .
H17 H 0.7245 0.7303 0.7500 0.061 Uiso 1 2 calc SR .
C7 C 0.3878(11) 0.4285(11) 0.5954(3) 0.0745(12) Uani 1 1 d . .
C16 C 0.5825(9) 0.6459(9) 0.7199(2) 0.057(2) Uani 1 1 d . .
H16 H 0.6251 0.6676 0.6987 0.068 Uiso 1 1 calc R .
C11 C 0.5051(11) 0.3356(9) 0.5990(3) 0.0745(12) Uani 1 1 d . .
H11 H 0.5438 0.3050 0.6125 0.089 Uiso 1 1 calc R .
C12 C 0.4487(11) 0.3891(11) 0.6147(3) 0.0745(12) Uani 1 1 d . .
H12 H 0.4525 0.3985 0.6392 0.089 Uiso 1 1 calc R .
C10 C 0.5029(11) 0.3282(10) 0.5618(3) 0.0745(12) Uani 1 1 d . .
H10 H 0.5410 0.2923 0.5506 0.089 Uiso 1 1 calc R .
C8 C 0.3963(11) 0.4248(11) 0.5601(2) 0.0745(12) Uani 1 1 d . .
H8 H 0.3646 0.4610 0.5459 0.089 Uiso 1 1 calc R .
C9 C 0.4521(11) 0.3677(10) 0.5441(3) 0.0745(12) Uani 1 1 d . .
H9 H 0.4501 0.3599 0.5196 0.089 Uiso 1 1 calc R .
Cl1 Cl 0.7580(8) 1.0970(16) 0.7871(2) 0.203(8) Uani 0.50 1 d PD 1
C18 C 0.816(4) 1.085(6) 0.7500 0.203(8) Uani 0.50 2 d SPD 1
H18A H 0.8114 1.0081 0.7500 0.243 Uiso 0.50 2 calc SPR 1
H18B H 0.8995 1.1457 0.7500 0.243 Uiso 0.50 2 calc SPR 1
C3 C 0.1614(11) 0.3712(11) 0.6183(4) 0.0990(18) Uani 1 1 d . .
C1 C 0.1327(12) 0.2838(9) 0.6429(4) 0.0990(18) Uani 1 1 d . .
H1 H 0.1910 0.2880 0.6582 0.119 Uiso 1 1 calc R .
C5 C 0.0833(11) 0.3666(11) 0.5955(5) 0.0990(18) Uani 1 1 d . .
H5 H 0.1048 0.4343 0.5818 0.119 Uiso 1 1 calc R .
C2 C 0.0214(11) 0.1924(11) 0.6450(5) 0.0990(18) Uani 1 1 d . .
H2 H -0.0002 0.1363 0.6630 0.119 Uiso 1 1 calc R .
C4 C -0.0292(12) 0.2690(10) 0.5902(5) 0.0990(18) Uani 1 1 d . .
H4 H -0.0784 0.2585 0.5709 0.119 Uiso 1 1 calc R .
C6 C -0.0601(11) 0.1819(10) 0.6204(4) 0.0990(18) Uani 1 1 d . .
H6 H -0.1381 0.1186 0.6223 0.119 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
P1 Cu1 P1 107.11(6) 3_565 2_665
P1 Cu1 P1 107.11(6) 3_565 .
P1 Cu1 P1 107.11(6) 2_665 .
P1 Cu1 I1 111.74(5) 3_565 .
P1 Cu1 I1 111.74(5) 2_665 .
P1 Cu1 I1 111.74(5) . .
C13 P1 C7 100.0(5) . .
C13 P1 C3 103.0(6) . .
C7 P1 C3 101.7(6) . .
C13 P1 Cu1 110.9(3) . .
C7 P1 Cu1 120.5(4) . .
C3 P1 Cu1 117.9(4) . .
C15 N1 C15 118.9(9) 4_556 .
C16 C15 N1 118.5(7) . .
C16 C15 C14 119.3(7) . .
N1 C15 C14 122.2(7) . .
C13 C14 C15 175.7(8) . .
C14 C13 P1 171.2(8) . .
C16 C17 C16 119.1(13) . 4_556
C16 C17 H17 120.5 . .
C16 C17 H17 120.5 4_556 .
C8 C7 C12 116.8(9) . .
C8 C7 P1 119.8(9) . .
C12 C7 P1 123.1(7) . .
C17 C16 C15 122.4(9) . .
C17 C16 H16 118.8 . .
C15 C16 H16 118.8 . .
C12 C11 C10 118.1(11) . .
C12 C11 H11 121.0 . .
C10 C11 H11 121.0 . .
C7 C12 C11 121.2(10) . .
C7 C12 H12 119.4 . .
C11 C12 H12 119.4 . .
C9 C10 C11 121.1(10) . .
C9 C10 H10 119.5 . .
C11 C10 H10 119.5 . .
C7 C8 C9 121.3(10) . .
C7 C8 H8 119.3 . .
C9 C8 H8 119.3 . .
C10 C9 C8 121.0(10) . .
C10 C9 H9 119.5 . .
C8 C9 H9 119.5 . .
Cl1 C18 Cl1 119(2) . 4_556
Cl1 C18 H18A 107.6 . .
Cl1 C18 H18A 107.6 4_556 .
Cl1 C18 H18B 107.6 . .
Cl1 C18 H18B 107.6 4_556 .
H18A C18 H18B 107.1 . .
C5 C3 C1 121.8(12) . .
C5 C3 P1 116.6(10) . .
C1 C3 P1 121.6(11) . .
C2 C1 C3 120.2(15) . .
C2 C1 H1 119.9 . .
C3 C1 H1 119.9 . .
C3 C5 C4 125.0(14) . .
C3 C5 H5 117.5 . .
C4 C5 H5 117.5 . .
C1 C2 C6 119.2(14) . .
C1 C2 H2 120.4 . .
C6 C2 H2 120.4 . .
C5 C4 C6 109.7(15) . .
C5 C4 H4 125.1 . .
C6 C4 H4 125.1 . .
C2 C6 C4 122.5(12) . .
C2 C6 H6 118.7 . .
C4 C6 H6 118.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Cu1 2.5731(15) .
Cu1 P1 2.278(2) 3_565
Cu1 P1 2.278(2) 2_665
Cu1 P1 2.278(2) .
P1 C13 1.762(8) .
P1 C7 1.812(10) .
P1 C3 1.838(12) .
N1 C15 1.401(8) 4_556
N1 C15 1.401(8) .
C15 C16 1.385(13) .
C15 C14 1.437(9) .
C14 C13 1.182(11) .
C17 C16 1.345(11) .
C17 C16 1.345(11) 4_556
C17 H17 0.9500 .
C7 C8 1.366(13) .
C7 C12 1.373(15) .
C16 H16 0.9500 .
C11 C12 1.394(14) .
C11 C10 1.434(15) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C10 C9 1.239(16) .
C10 H10 0.9500 .
C8 C9 1.430(14) .
C8 H8 0.9500 .
C9 H9 0.9500 .
Cl1 C18 1.663(19) .
C18 Cl1 1.663(19) 4_556
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C3 C5 1.33(2) .
C3 C1 1.390(18) .
C1 C2 1.359(17) .
C1 H1 0.9500 .
C5 C4 1.412(18) .
C5 H5 0.9500 .
C2 C6 1.39(2) .
C2 H2 0.9500 .
C4 C6 1.540(19) .
C4 H4 0.9500 .
C6 H6 0.9500 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 455 169 ' '
