#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:31:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179382 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/79/4327944.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_4327944
loop_
_publ_author_name
'Sandrine Perruchas'
'Nicolas Desboeufs'
'Sébastien Maron'
'Xavier F. Le Goff'
'Alexandre Fargues'
'Alain Garcia'
'Thierry Gacoin'
'Jean-Pierre Boilot'
_publ_contact_author_address
;Laboratoire DCPH
Ecole Polytechnique
Route de Saclay
F91128 Palaiseau
France
;
_publ_contact_author_email       xavier-frederic.legoff@polytechnique.edu
_publ_contact_author_fax         330169334440
_publ_contact_author_name        'Xavier F. Le Goff'
_publ_contact_author_phone       330169334413
_publ_section_title
;
 Siloxanol-Functionalized Copper Iodide Cluster as a Thermochromic
 Luminescent Building Block
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              794
_journal_page_last               798
_journal_paper_doi               10.1021/ic200672r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C56 H64 Cu4 I4 O10 P4 Si4, 4(C4 H8 O)'
_chemical_formula_sum            'C72 H96 Cu4 I4 O14 P4 Si4'
_chemical_formula_weight         2183.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-12-22
_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                   22.616(1)
_cell_length_b                   22.616(1)
_cell_length_c                   16.932(1)
_cell_measurement_reflns_used    4615
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     8660.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  KappaCCD
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10900
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    2.580
_exptl_absorpt_correction_T_max  0.6006
_exptl_absorpt_correction_T_min  0.5319
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       Block
_exptl_crystal_F_000             4336
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.754
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0351
_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)+(0.0597P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                3665
_reflns_number_total             4618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200672r_si_002.cif
_cod_data_source_block           sp3-26a
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4327944
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
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 -0.090095(10) 0.205350(11) 0.215153(14) 0.02843(11) Uani 1 1 d .
Cu1 Cu 0.02485(2) 0.19564(2) 0.18309(3) 0.02957(14) Uani 1 1 d .
P1 P 0.06740(4) 0.13199(4) 0.26701(6) 0.0256(2) Uani 1 1 d .
Si1 Si -0.00361(5) 0.17900(5) 0.50829(6) 0.0277(2) Uani 1 1 d .
O1 O 0.0000 0.2500 0.5120(2) 0.0443(11) Uani 1 2 d S
O2 O -0.06625(14) 0.15689(14) 0.54291(16) 0.0379(7) Uani 1 1 d .
H2O H -0.073(2) 0.163(2) 0.585(3) 0.057 Uiso 1 1 d .
O3 O 0.05218(14) 0.15453(14) 0.56045(19) 0.0373(7) Uani 1 1 d .
H3O H 0.073(2) 0.123(2) 0.551(3) 0.056 Uiso 1 1 d .
C1 C 0.06349(18) 0.15542(17) 0.3710(2) 0.0296(9) Uani 1 1 d .
H1A H 0.0907 0.1307 0.4026 0.036 Uiso 1 1 calc R
H1B H 0.0771 0.1969 0.3751 0.036 Uiso 1 1 calc R
C2 C 0.00111(17) 0.15071(18) 0.4059(2) 0.0320(9) Uani 1 1 d .
H2A H -0.0114 0.1088 0.4052 0.038 Uiso 1 1 calc R
H2B H -0.0267 0.1733 0.3722 0.038 Uiso 1 1 calc R
C3 C 0.14654(17) 0.12353(17) 0.2516(2) 0.0272(8) Uani 1 1 d .
C4 C 0.18711(19) 0.1603(2) 0.2888(2) 0.0391(10) Uani 1 1 d .
H4 H 0.1736 0.1888 0.3258 0.047 Uiso 1 1 calc R
C5 C 0.2469(2) 0.1558(2) 0.2726(3) 0.0498(12) Uani 1 1 d .
H5 H 0.2739 0.1819 0.2978 0.060 Uiso 1 1 calc R
C6 C 0.2671(2) 0.1152(2) 0.2219(3) 0.0522(13) Uani 1 1 d .
H6 H 0.3084 0.1112 0.2133 0.063 Uiso 1 1 calc R
C7 C 0.2281(2) 0.0791(2) 0.1822(3) 0.0570(14) Uani 1 1 d .
H7 H 0.2424 0.0516 0.1443 0.068 Uiso 1 1 calc R
C8 C 0.1676(2) 0.0829(2) 0.1974(3) 0.0475(12) Uani 1 1 d .
H8 H 0.1408 0.0576 0.1705 0.057 Uiso 1 1 calc R
C9 C 0.04070(17) 0.05634(17) 0.2650(2) 0.0292(8) Uani 1 1 d .
C10 C -0.0041(2) 0.0403(2) 0.2147(2) 0.0406(10) Uani 1 1 d .
H10 H -0.0213 0.0695 0.1816 0.049 Uiso 1 1 calc R
C11 C -0.0249(2) -0.0175(2) 0.2107(3) 0.0565(14) Uani 1 1 d .
H11 H -0.0561 -0.0275 0.1756 0.068 Uiso 1 1 calc R
C12 C -0.0001(3) -0.0601(2) 0.2580(3) 0.0537(14) Uani 1 1 d .
H12 H -0.0132 -0.0999 0.2543 0.064 Uiso 1 1 calc R
C13 C 0.0439(2) -0.0451(2) 0.3111(3) 0.0551(13) Uani 1 1 d .
H13 H 0.0602 -0.0743 0.3451 0.066 Uiso 1 1 calc R
C14 C 0.0642(2) 0.01298(19) 0.3143(3) 0.0416(10) Uani 1 1 d .
H14 H 0.0946 0.0232 0.3507 0.050 Uiso 1 1 calc R
O4 O 0.10607(17) 0.05181(15) 0.5179(2) 0.0592(9) Uani 1 1 d .
C15 C 0.0818(2) -0.0022(2) 0.5469(3) 0.0580(14) Uani 1 1 d .
H15A H 0.0556 -0.0204 0.5069 0.070 Uiso 1 1 calc R
H15B H 0.0586 0.0049 0.5957 0.070 Uiso 1 1 calc R
C16 C 0.1342(2) -0.0418(3) 0.5638(4) 0.0681(16) Uani 1 1 d .
H16A H 0.1235 -0.0841 0.5590 0.082 Uiso 1 1 calc R
H16B H 0.1505 -0.0344 0.6172 0.082 Uiso 1 1 calc R
C17 C 0.1772(3) -0.0230(3) 0.4997(3) 0.0696(17) Uani 1 1 d .
H17A H 0.1665 -0.0400 0.4477 0.084 Uiso 1 1 calc R
H17B H 0.2184 -0.0341 0.5130 0.084 Uiso 1 1 calc R
C18 C 0.1682(2) 0.0439(2) 0.5016(4) 0.0647(15) Uani 1 1 d .
H18A H 0.1927 0.0621 0.5435 0.078 Uiso 1 1 calc R
H18B H 0.1789 0.0618 0.4502 0.078 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'
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'
O O 0.0106 0.0060 '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'
Si Si 0.0817 0.0704 '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
Cu1 I1 Cu1 61.825(17) . 14
Cu1 I1 Cu1 60.058(18) . 7_454
Cu1 I1 Cu1 60.910(17) 14 7_454
P1 Cu1 I1 110.05(3) . .
P1 Cu1 I1 109.22(3) . 12_666
I1 Cu1 I1 112.294(18) . 12_666
P1 Cu1 Cu1 139.74(3) . 7_454
I1 Cu1 Cu1 61.280(18) . 7_454
I1 Cu1 Cu1 110.146(11) 12_666 7_454
P1 Cu1 I1 99.69(3) . 7_454
I1 Cu1 I1 114.727(18) . 7_454
I1 Cu1 I1 110.075(17) 12_666 7_454
Cu1 Cu1 I1 58.664(18) 7_454 7_454
P1 Cu1 Cu1 140.37(3) . 12_666
I1 Cu1 Cu1 109.247(16) . 12_666
I1 Cu1 Cu1 58.909(19) 12_666 12_666
Cu1 Cu1 Cu1 60.476(10) 7_454 12_666
I1 Cu1 Cu1 58.443(15) 7_454 12_666
P1 Cu1 Cu1 153.11(4) . 14
I1 Cu1 Cu1 59.266(15) . 14
I1 Cu1 Cu1 60.648(19) 12_666 14
Cu1 Cu1 Cu1 60.476(10) 7_454 14
I1 Cu1 Cu1 107.183(16) 7_454 14
Cu1 Cu1 Cu1 59.05(2) 12_666 14
C9 P1 C3 103.03(18) . .
C9 P1 C1 105.84(17) . .
C3 P1 C1 102.39(18) . .
C9 P1 Cu1 116.83(13) . .
C3 P1 Cu1 113.55(12) . .
C1 P1 Cu1 113.66(13) . .
O1 Si1 O2 109.86(14) . .
O1 Si1 O3 106.09(15) . .
O2 Si1 O3 112.11(17) . .
O1 Si1 C2 112.25(19) . .
O2 Si1 C2 106.50(17) . .
O3 Si1 C2 110.12(17) . .
Si1 O1 Si1 175.5(3) 7_454 .
Si1 O2 H2O 118(4) . .
Si1 O3 H3O 127(3) . .
C2 C1 P1 113.1(3) . .
C2 C1 H1A 109.0 . .
P1 C1 H1A 109.0 . .
C2 C1 H1B 109.0 . .
P1 C1 H1B 109.0 . .
H1A C1 H1B 107.8 . .
C1 C2 Si1 113.0(3) . .
C1 C2 H2A 109.0 . .
Si1 C2 H2A 109.0 . .
C1 C2 H2B 109.0 . .
Si1 C2 H2B 109.0 . .
H2A C2 H2B 107.8 . .
C8 C3 C4 118.1(4) . .
C8 C3 P1 120.2(3) . .
C4 C3 P1 121.5(3) . .
C5 C4 C3 120.8(4) . .
C5 C4 H4 119.6 . .
C3 C4 H4 119.6 . .
C6 C5 C4 120.7(5) . .
C6 C5 H5 119.7 . .
C4 C5 H5 119.7 . .
C5 C6 C7 120.1(5) . .
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 . .
C6 C7 C8 120.1(5) . .
C6 C7 H7 120.0 . .
C8 C7 H7 120.0 . .
C3 C8 C7 120.1(4) . .
C3 C8 H8 120.0 . .
C7 C8 H8 120.0 . .
C10 C9 C14 117.9(4) . .
C10 C9 P1 120.4(3) . .
C14 C9 P1 121.7(3) . .
C9 C10 C11 121.8(4) . .
C9 C10 H10 119.1 . .
C11 C10 H10 119.1 . .
C12 C11 C10 119.5(5) . .
C12 C11 H11 120.2 . .
C10 C11 H11 120.2 . .
C11 C12 C13 120.1(4) . .
C11 C12 H12 119.9 . .
C13 C12 H12 119.9 . .
C12 C13 C14 119.6(5) . .
C12 C13 H13 120.2 . .
C14 C13 H13 120.2 . .
C13 C14 C9 120.9(5) . .
C13 C14 H14 119.5 . .
C9 C14 H14 119.5 . .
C15 O4 C18 109.5(4) . .
O4 C15 C16 105.7(4) . .
O4 C15 H15A 110.6 . .
C16 C15 H15A 110.6 . .
O4 C15 H15B 110.6 . .
C16 C15 H15B 110.6 . .
H15A C15 H15B 108.7 . .
C15 C16 C17 101.7(4) . .
C15 C16 H16A 111.4 . .
C17 C16 H16A 111.4 . .
C15 C16 H16B 111.4 . .
C17 C16 H16B 111.4 . .
H16A C16 H16B 109.3 . .
C16 C17 C18 100.1(4) . .
C16 C17 H17A 111.7 . .
C18 C17 H17A 111.7 . .
C16 C17 H17B 111.7 . .
C18 C17 H17B 111.7 . .
H17A C17 H17B 109.5 . .
O4 C18 C17 104.9(4) . .
O4 C18 H18A 110.8 . .
C17 C18 H18A 110.8 . .
O4 C18 H18B 110.8 . .
C17 C18 H18B 110.8 . .
H18A C18 H18B 108.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Cu1 2.6648(5) .
I1 Cu1 2.6747(5) 14
I1 Cu1 2.7361(6) 7_454
Cu1 P1 2.2398(11) .
Cu1 I1 2.6748(5) 12_666
Cu1 Cu1 2.7035(10) 7_454
Cu1 I1 2.7360(6) 7_454
Cu1 Cu1 2.7430(8) 12_666
Cu1 Cu1 2.7431(8) 14
P1 C9 1.815(4) .
P1 C3 1.819(4) .
P1 C1 1.841(4) .
Si1 O1 1.6091(11) .
Si1 O2 1.612(3) .
Si1 O3 1.637(3) .
Si1 C2 1.851(4) .
O1 Si1 1.6090(11) 7_454
O2 H2O 0.74(5) .
O3 H3O 0.87(5) .
C1 C2 1.533(5) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C8 1.383(6) .
C3 C4 1.389(6) .
C4 C5 1.383(6) .
C4 H4 0.9500 .
C5 C6 1.339(7) .
C5 H5 0.9500 .
C6 C7 1.377(7) .
C6 H6 0.9500 .
C7 C8 1.395(6) .
C7 H7 0.9500 .
C8 H8 0.9500 .
C9 C10 1.373(6) .
C9 C14 1.393(6) .
C10 C11 1.393(6) .
C10 H10 0.9500 .
C11 C12 1.372(7) .
C11 H11 0.9500 .
C12 C13 1.383(7) .
C12 H12 0.9500 .
C13 C14 1.393(6) .
C13 H13 0.9500 .
C14 H14 0.9500 .
O4 C15 1.427(6) .
O4 C18 1.444(6) .
C15 C16 1.512(7) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 C17 1.519(8) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.527(8) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
