#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305546.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_4305546
loop_
_publ_author_name
'Marlyn Rivera-Carrillo'
'Indranil Chakraborty'
'Gellert Mezei'
'Richard D. Webster'
'Raphael G. Raptis'
_publ_section_title
;
Tuning of the [Cu3(μ-O)]4+/5+ Redox Couple: Spectroscopic Evidence of
Charge Delocalization in the Mixed-Valent [Cu3(μ-O)]5+ Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7644
_journal_page_last               7650
_journal_paper_doi               10.1021/ic800531y
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         (PPN)3[Cu3(mu-O)(mu-4-Cl-pz)3Cl3]Cl(H2O)
_chemical_formula_sum            'C117 H98 Cl7 Cu3 N9 O2 P6'
_chemical_formula_weight         2286.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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            3
_cell_length_a                   22.8405(16)
_cell_length_b                   22.8405(16)
_cell_length_c                   17.9558(18)
_cell_measurement_temperature    293(2)
_cell_volume                     8112.3(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11980
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3525
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.053(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4559
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0383
_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)+(0.0502P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                3628
_reflns_number_total             4559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800531y-file001_2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4305546
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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
Cu1 Cu 0.57643(3) 0.26097(3) 0.27503(4) 0.0438(2) Uani 1 1 d . . .
Cl1 Cl 0.46980(8) 0.17772(9) 0.24274(12) 0.0757(6) Uani 1 1 d . . .
Cl2 Cl 0.60841(11) 0.03617(9) 0.36406(11) 0.0757(6) Uani 1 1 d . . .
Cl3 Cl 0.3333 0.6667 0.1140(3) 0.1392(18) Uani 1 3 d S . .
P1 P 0.11717(7) 0.28157(8) 0.45309(8) 0.0395(4) Uani 1 1 d . . .
P2 P 0.14464(8) 0.23954(7) 0.30856(8) 0.0394(4) Uani 1 1 d . . .
O1 O 0.6667 0.3333 0.2626(4) 0.054(2) Uani 1 3 d S . .
O2 O 0.6667 0.3333 0.1063(6) 0.118(4) Uani 1 3 d S . .
H2O H 0.6667 0.3333 0.1533 0.142 Uiso 1 3 d SR . .
N1 N 0.6083(2) 0.1973(2) 0.2950(3) 0.0432(12) Uani 1 1 d . . .
N2 N 0.5453(2) 0.3245(2) 0.2988(3) 0.0461(12) Uani 1 1 d . . .
N3 N 0.1167(2) 0.2337(2) 0.3898(2) 0.0473(13) Uani 1 1 d . . .
C1 C 0.5753(3) 0.1324(3) 0.3157(3) 0.0501(16) Uani 1 1 d . . .
H1 H 0.5286 0.1045 0.3171 0.060 Uiso 1 1 calc R . .
C2 C 0.6226(3) 0.1138(3) 0.3345(3) 0.0486(16) Uani 1 1 d . . .
C3 C 0.6855(4) 0.1710(3) 0.3231(3) 0.0533(17) Uani 1 1 d . . .
H3 H 0.7272 0.1741 0.3309 0.064 Uiso 1 1 calc R . .
C4 C 0.0972(3) 0.2348(3) 0.5390(3) 0.0435(15) Uani 1 1 d . . .
C5 C 0.0683(3) 0.1646(3) 0.5371(4) 0.0528(17) Uani 1 1 d . . .
H5 H 0.0625 0.1428 0.4917 0.063 Uiso 1 1 calc R . .
C6 C 0.0484(3) 0.1278(4) 0.6011(5) 0.0618(19) Uani 1 1 d . . .
H6 H 0.0292 0.0810 0.5996 0.074 Uiso 1 1 calc R . .
C7 C 0.0571(4) 0.1603(5) 0.6678(5) 0.080(2) Uani 1 1 d . . .
H7 H 0.0437 0.1350 0.7114 0.096 Uiso 1 1 calc R . .
C8 C 0.0846(4) 0.2282(5) 0.6720(4) 0.076(2) Uani 1 1 d . . .
H8 H 0.0896 0.2493 0.7178 0.092 Uiso 1 1 calc R . .
C9 C 0.1050(3) 0.2658(3) 0.6067(4) 0.0594(18) Uani 1 1 d . . .
H9 H 0.1243 0.3126 0.6089 0.071 Uiso 1 1 calc R . .
C10 C 0.1976(3) 0.3575(3) 0.4639(3) 0.0418(15) Uani 1 1 d . . .
C11 C 0.2507(3) 0.3509(3) 0.4905(4) 0.0555(17) Uani 1 1 d . . .
H11 H 0.2430 0.3089 0.5065 0.067 Uiso 1 1 calc R . .
C12 C 0.3147(4) 0.4060(4) 0.4934(4) 0.072(2) Uani 1 1 d . . .
H12 H 0.3505 0.4011 0.5104 0.086 Uiso 1 1 calc R . .
C13 C 0.3258(4) 0.4679(4) 0.4713(4) 0.069(2) Uani 1 1 d . . .
H13 H 0.3690 0.5053 0.4743 0.083 Uiso 1 1 calc R . .
C14 C 0.2736(4) 0.4753(4) 0.4448(4) 0.070(2) Uani 1 1 d . . .
H14 H 0.2818 0.5176 0.4294 0.084 Uiso 1 1 calc R . .
C15 C 0.2088(3) 0.4203(3) 0.4408(3) 0.0549(17) Uani 1 1 d . . .
H15 H 0.1733 0.4253 0.4230 0.066 Uiso 1 1 calc R . .
C16 C 0.0539(3) 0.3054(3) 0.4388(3) 0.0414(15) Uani 1 1 d . . .
C17 C 0.0484(3) 0.3496(4) 0.4882(4) 0.0636(19) Uani 1 1 d . . .
H17 H 0.0774 0.3662 0.5289 0.076 Uiso 1 1 calc R . .
C18 C 0.0008(4) 0.3689(4) 0.4775(4) 0.074(2) Uani 1 1 d . . .
H18 H -0.0020 0.3992 0.5098 0.088 Uiso 1 1 calc R . .
C19 C -0.0428(4) 0.3421(4) 0.4177(5) 0.076(2) Uani 1 1 d . . .
H19 H -0.0758 0.3540 0.4103 0.091 Uiso 1 1 calc R . .
C20 C -0.0382(3) 0.2990(4) 0.3697(4) 0.069(2) Uani 1 1 d . . .
H20 H -0.0676 0.2820 0.3294 0.083 Uiso 1 1 calc R . .
C21 C 0.0091(3) 0.2803(3) 0.3800(4) 0.0586(18) Uani 1 1 d . . .
H21 H 0.0114 0.2502 0.3469 0.070 Uiso 1 1 calc R . .
C22 C 0.2052(3) 0.2118(3) 0.3048(4) 0.0437(15) Uani 1 1 d . . .
C23 C 0.2328(3) 0.2086(3) 0.2382(4) 0.0566(18) Uani 1 1 d . . .
H23 H 0.2198 0.2213 0.1948 0.068 Uiso 1 1 calc R . .
C24 C 0.2797(4) 0.1870(3) 0.2341(5) 0.070(2) Uani 1 1 d . . .
H24 H 0.2970 0.1840 0.1883 0.084 Uiso 1 1 calc R . .
C25 C 0.2999(4) 0.1702(4) 0.2978(6) 0.086(3) Uani 1 1 d . . .
H25 H 0.3325 0.1573 0.2960 0.103 Uiso 1 1 calc R . .
C26 C 0.2730(5) 0.1722(5) 0.3628(6) 0.109(3) Uani 1 1 d . . .
H26 H 0.2865 0.1598 0.4060 0.131 Uiso 1 1 calc R . .
C27 C 0.2247(4) 0.1925(4) 0.3673(4) 0.086(3) Uani 1 1 d . . .
H27 H 0.2059 0.1929 0.4131 0.103 Uiso 1 1 calc R . .
C28 C 0.1848(3) 0.3240(3) 0.2699(3) 0.0375(14) Uani 1 1 d . . .
C29 C 0.2546(3) 0.3658(3) 0.2767(3) 0.0497(17) Uani 1 1 d . . .
H29 H 0.2810 0.3485 0.2951 0.060 Uiso 1 1 calc R . .
C30 C 0.2841(3) 0.4322(3) 0.2564(4) 0.0551(18) Uani 1 1 d . . .
H30 H 0.3304 0.4603 0.2623 0.066 Uiso 1 1 calc R . .
C31 C 0.2463(4) 0.4577(3) 0.2275(4) 0.065(2) Uani 1 1 d . . .
H31 H 0.2669 0.5026 0.2122 0.079 Uiso 1 1 calc R . .
C32 C 0.1773(4) 0.4167(3) 0.2210(4) 0.0645(19) Uani 1 1 d . . .
H32 H 0.1512 0.4340 0.2021 0.077 Uiso 1 1 calc R . .
C33 C 0.1471(3) 0.3500(3) 0.2427(3) 0.0508(16) Uani 1 1 d . . .
H33 H 0.1005 0.3225 0.2385 0.061 Uiso 1 1 calc R . .
C34 C 0.0759(3) 0.1836(3) 0.2493(3) 0.0417(15) Uani 1 1 d . . .
C35 C 0.0229(3) 0.1278(3) 0.2811(4) 0.0581(18) Uani 1 1 d . . .
H35 H 0.0210 0.1222 0.3325 0.070 Uiso 1 1 calc R . .
C36 C -0.0281(4) 0.0796(4) 0.2364(5) 0.078(2) Uani 1 1 d . . .
H36 H -0.0630 0.0406 0.2575 0.094 Uiso 1 1 calc R . .
C37 C -0.0268(4) 0.0897(4) 0.1611(5) 0.077(2) Uani 1 1 d . . .
H37 H -0.0624 0.0585 0.1318 0.093 Uiso 1 1 calc R . .
C38 C 0.0253(4) 0.1442(4) 0.1288(4) 0.069(2) Uani 1 1 d . . .
H38 H 0.0264 0.1495 0.0773 0.082 Uiso 1 1 calc R . .
C39 C 0.0776(3) 0.1925(3) 0.1727(4) 0.0548(17) Uani 1 1 d . . .
H39 H 0.1134 0.2305 0.1508 0.066 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
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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'
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'
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
O1 Cu1 N2 91.07(15) . . ?
O1 Cu1 N1 91.33(15) . . ?
N2 Cu1 N1 156.9(2) . . ?
O1 Cu1 Cl1 158.6(2) . . ?
N2 Cu1 Cl1 92.35(15) . . ?
N1 Cu1 Cl1 93.76(15) . . ?
N3 P1 C16 112.3(3) . . ?
N3 P1 C4 107.1(3) . . ?
C16 P1 C4 107.3(3) . . ?
N3 P1 C10 113.4(3) . . ?
C16 P1 C10 108.1(3) . . ?
C4 P1 C10 108.3(3) . . ?
N3 P2 C22 111.0(3) . . ?
N3 P2 C34 108.5(3) . . ?
C22 P2 C34 106.3(3) . . ?
N3 P2 C28 114.5(2) . . ?
C22 P2 C28 107.1(3) . . ?
C34 P2 C28 109.2(3) . . ?
Cu1 O1 Cu1 118.65(9) 2_655 . ?
Cu1 O1 Cu1 118.65(9) 2_655 3_665 ?
Cu1 O1 Cu1 118.65(9) . 3_665 ?
C1 N1 N2 109.1(5) . 2_655 ?
C1 N1 Cu1 131.4(4) . . ?
N2 N1 Cu1 119.0(4) 2_655 . ?
C3 N2 N1 108.8(5) 3_665 3_665 ?
C3 N2 Cu1 131.4(4) 3_665 . ?
N1 N2 Cu1 119.7(3) 3_665 . ?
P2 N3 P1 138.6(3) . . ?
N1 C1 C2 108.2(5) . . ?
C1 C2 C3 105.9(5) . . ?
C1 C2 Cl2 128.1(5) . . ?
C3 C2 Cl2 125.9(5) . . ?
N2 C3 C2 108.0(6) 2_655 . ?
C9 C4 C5 118.6(6) . . ?
C9 C4 P1 121.6(5) . . ?
C5 C4 P1 119.7(5) . . ?
C6 C5 C4 120.7(7) . . ?
C5 C6 C7 119.3(7) . . ?
C8 C7 C6 121.9(7) . . ?
C7 C8 C9 118.8(7) . . ?
C4 C9 C8 120.8(7) . . ?
C11 C10 C15 119.9(6) . . ?
C11 C10 P1 117.4(5) . . ?
C15 C10 P1 122.4(5) . . ?
C12 C11 C10 120.3(7) . . ?
C13 C12 C11 120.0(7) . . ?
C12 C13 C14 120.5(7) . . ?
C13 C14 C15 120.4(7) . . ?
C14 C15 C10 118.9(6) . . ?
C21 C16 C17 118.1(6) . . ?
C21 C16 P1 121.6(5) . . ?
C17 C16 P1 120.2(4) . . ?
C18 C17 C16 121.0(6) . . ?
C17 C18 C19 118.4(7) . . ?
C20 C19 C18 121.1(7) . . ?
C19 C20 C21 120.5(7) . . ?
C20 C21 C16 120.9(7) . . ?
C27 C22 C23 118.1(6) . . ?
C27 C22 P2 121.4(5) . . ?
C23 C22 P2 120.5(5) . . ?
C22 C23 C24 121.4(6) . . ?
C25 C24 C23 119.1(7) . . ?
C26 C25 C24 120.1(8) . . ?
C25 C26 C27 121.1(8) . . ?
C22 C27 C26 120.1(8) . . ?
C33 C28 C29 119.3(6) . . ?
C33 C28 P2 120.7(5) . . ?
C29 C28 P2 119.5(4) . . ?
C30 C29 C28 119.7(6) . . ?
C31 C30 C29 120.7(6) . . ?
C30 C31 C32 119.6(6) . . ?
C33 C32 C31 119.9(6) . . ?
C28 C33 C32 120.6(6) . . ?
C35 C34 C39 119.9(6) . . ?
C35 C34 P2 117.8(5) . . ?
C39 C34 P2 122.2(4) . . ?
C34 C35 C36 119.7(7) . . ?
C37 C36 C35 120.0(7) . . ?
C38 C37 C36 120.9(7) . . ?
C37 C38 C39 119.8(7) . . ?
C34 C39 C38 119.6(6) . . ?
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
Cu1 O1 1.9033(11) . ?
Cu1 N2 1.957(5) . ?
Cu1 N1 1.958(5) . ?
Cu1 Cl1 2.2919(18) . ?
Cl2 C2 1.720(6) . ?
P1 N3 1.574(5) . ?
P1 C16 1.800(6) . ?
P1 C4 1.799(6) . ?
P1 C10 1.799(6) . ?
P2 N3 1.571(5) . ?
P2 C22 1.789(6) . ?
P2 C34 1.796(6) . ?
P2 C28 1.809(6) . ?
O1 Cu1 1.9033(11) 2_655 ?
O1 Cu1 1.9033(11) 3_665 ?
N1 C1 1.336(7) . ?
N1 N2 1.349(6) 2_655 ?
N2 C3 1.339(7) 3_665 ?
N2 N1 1.349(6) 3_665 ?
C1 C2 1.385(8) . ?
C2 C3 1.392(8) . ?
C3 N2 1.339(7) 2_655 ?
C4 C9 1.374(8) . ?
C4 C5 1.396(8) . ?
C5 C6 1.362(9) . ?
C6 C7 1.370(11) . ?
C7 C8 1.354(10) . ?
C8 C9 1.389(9) . ?
C10 C11 1.380(8) . ?
C10 C15 1.388(8) . ?
C11 C12 1.373(9) . ?
C12 C13 1.365(10) . ?
C13 C14 1.371(10) . ?
C14 C15 1.384(9) . ?
C16 C21 1.379(8) . ?
C16 C17 1.395(8) . ?
C17 C18 1.376(9) . ?
C18 C19 1.382(10) . ?
C19 C20 1.351(10) . ?
C20 C21 1.358(9) . ?
C22 C27 1.358(9) . ?
C22 C23 1.371(8) . ?
C23 C24 1.388(9) . ?
C24 C25 1.359(11) . ?
C25 C26 1.330(12) . ?
C26 C27 1.397(10) . ?
C28 C33 1.357(8) . ?
C28 C29 1.396(8) . ?
C29 C30 1.367(8) . ?
C30 C31 1.363(9) . ?
C31 C32 1.377(9) . ?
C32 C33 1.377(8) . ?
C34 C35 1.369(8) . ?
C34 C39 1.388(8) . ?
C35 C36 1.390(10) . ?
C36 C37 1.368(10) . ?
C37 C38 1.351(10) . ?
C38 C39 1.396(9) . ?
