#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305548.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_4305548
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-NO2-pz)3Cl3]Cl
_chemical_formula_sum            'C117 H96 Cl4 Cu3 N12 O7 P6'
_chemical_formula_weight         2300.30
_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                   22.944(2)
_cell_length_b                   22.944(2)
_cell_length_c                   17.826(3)
_cell_measurement_temperature    293(2)
_cell_volume                     8126.9(17)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1058
_diffrn_reflns_av_sigmaI/netI    0.1398
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14319
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            VIOLET
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3549
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(3)
_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     448
_refine_ls_number_reflns         4680
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0572
_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)+(0.0648P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1452
_reflns_number_gt                2782
_reflns_number_total             4680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800531y-file001_4.cif
_cod_data_source_block           7
_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               4305548
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 0.26011(6) 0.57761(6) 0.10308(7) 0.0434(4) Uani 1 1 d . . .
Cl1 Cl 0.17545(15) 0.47263(15) 0.1337(2) 0.0722(10) Uani 1 1 d . . .
Cl2 Cl 0.0000 0.0000 0.9321(4) 0.122(3) Uani 1 3 d S . .
P1 P 0.23896(14) 0.14389(14) 1.06623(16) 0.0378(7) Uani 1 1 d . . .
P2 P 0.27857(14) 0.11477(14) 0.92002(16) 0.0400(8) Uani 1 1 d . . .
O1 O 0.3333 0.6667 0.1063(9) 0.071(5) Uani 1 3 d S . .
O2 O 0.3332(6) 0.3822(5) 0.0038(6) 0.104(4) Uani 1 1 d . . .
O3 O 0.4401(6) 0.4496(6) 0.0056(6) 0.104(4) Uani 1 1 d . . .
N1 N 0.3215(4) 0.5442(4) 0.0799(5) 0.044(2) Uani 1 1 d . . .
N2 N 0.1967(4) 0.6098(4) 0.0819(5) 0.043(2) Uani 1 1 d . . .
N3 N 0.3845(7) 0.4386(6) 0.0145(6) 0.066(3) Uani 1 1 d . . .
N4 N 0.2324(4) 0.1151(4) 0.9840(5) 0.045(2) Uani 1 1 d . . .
C1 C 0.3112(6) 0.4840(6) 0.0553(6) 0.053(3) Uani 1 1 d . . .
H1 H 0.2694 0.4454 0.0493 0.064 Uiso 1 1 calc R . .
C2 C 0.3720(6) 0.4888(6) 0.0409(6) 0.046(3) Uani 1 1 d . . .
C3 C 0.4210(6) 0.5543(6) 0.0599(6) 0.046(3) Uani 1 1 d . . .
H3 H 0.4674 0.5719 0.0574 0.055 Uiso 1 1 calc R . .
C4 C 0.2323(6) 0.0931(5) 0.8352(6) 0.041(3) Uani 1 1 d . . .
C5 C 0.2615(6) 0.0976(6) 0.7678(8) 0.057(3) Uani 1 1 d . . .
H5 H 0.3077 0.1143 0.7655 0.068 Uiso 1 1 calc R . .
C6 C 0.2250(8) 0.0782(6) 0.7037(8) 0.075(4) Uani 1 1 d . . .
H6 H 0.2461 0.0826 0.6579 0.091 Uiso 1 1 calc R . .
C7 C 0.1550(9) 0.0515(7) 0.7067(9) 0.078(4) Uani 1 1 d . . .
H7 H 0.1298 0.0371 0.6628 0.093 Uiso 1 1 calc R . .
C8 C 0.1239(6) 0.0467(6) 0.7727(9) 0.062(4) Uani 1 1 d . . .
H8 H 0.0778 0.0299 0.7751 0.074 Uiso 1 1 calc R . .
C9 C 0.1633(6) 0.0675(5) 0.8366(7) 0.055(3) Uani 1 1 d . . .
H9 H 0.1426 0.0643 0.8825 0.066 Uiso 1 1 calc R . .
C10 C 0.3519(5) 0.1933(5) 0.9088(6) 0.039(3) Uani 1 1 d . . .
C11 C 0.3449(6) 0.2449(6) 0.8838(7) 0.059(3) Uani 1 1 d . . .
H11 H 0.3025 0.2364 0.8687 0.070 Uiso 1 1 calc R . .
C12 C 0.3985(8) 0.3102(7) 0.8799(7) 0.072(4) Uani 1 1 d . . .
H12 H 0.3923 0.3445 0.8610 0.086 Uiso 1 1 calc R . .
C13 C 0.4578(8) 0.3231(6) 0.9031(7) 0.066(4) Uani 1 1 d . . .
H13 H 0.4933 0.3673 0.9037 0.079 Uiso 1 1 calc R . .
C14 C 0.4680(6) 0.2714(8) 0.9270(7) 0.070(4) Uani 1 1 d . . .
H14 H 0.5108 0.2805 0.9413 0.085 Uiso 1 1 calc R . .
C15 C 0.4142(6) 0.2057(6) 0.9296(6) 0.061(4) Uani 1 1 d . . .
H15 H 0.4206 0.1708 0.9453 0.073 Uiso 1 1 calc R . .
C16 C 0.3045(5) 0.0525(5) 0.9349(6) 0.036(3) Uani 1 1 d . . .
C17 C 0.3469(6) 0.0472(6) 0.8869(7) 0.061(4) Uani 1 1 d . . .
H17 H 0.3627 0.0755 0.8454 0.073 Uiso 1 1 calc R . .
C18 C 0.3673(6) 0.0012(7) 0.8981(8) 0.069(4) Uani 1 1 d . . .
H18 H 0.3960 -0.0027 0.8643 0.083 Uiso 1 1 calc R . .
C19 C 0.3440(7) -0.0395(6) 0.9609(9) 0.067(4) Uani 1 1 d . . .
H19 H 0.3588 -0.0697 0.9709 0.081 Uiso 1 1 calc R . .
C20 C 0.3001(7) -0.0356(6) 1.0077(8) 0.072(4) Uani 1 1 d . . .
H20 H 0.2831 -0.0647 1.0484 0.087 Uiso 1 1 calc R . .
C21 C 0.2810(6) 0.0090(5) 0.9961(6) 0.054(3) Uani 1 1 d . . .
H21 H 0.2513 0.0115 1.0295 0.065 Uiso 1 1 calc R . .
C22 C 0.1849(6) 0.0758(5) 1.1261(6) 0.043(3) Uani 1 1 d . . .
C23 C 0.1282(6) 0.0225(6) 1.0937(8) 0.062(4) Uani 1 1 d . . .
H23 H 0.1218 0.0210 1.0421 0.075 Uiso 1 1 calc R . .
C24 C 0.0827(6) -0.0266(7) 1.1376(10) 0.080(4) Uani 1 1 d . . .
H24 H 0.0439 -0.0615 1.1163 0.096 Uiso 1 1 calc R . .
C25 C 0.0927(7) -0.0264(7) 1.2149(9) 0.075(4) Uani 1 1 d . . .
H25 H 0.0610 -0.0609 1.2451 0.091 Uiso 1 1 calc R . .
C26 C 0.1490(8) 0.0246(7) 1.2451(8) 0.073(4) Uani 1 1 d . . .
H26 H 0.1571 0.0244 1.2962 0.087 Uiso 1 1 calc R . .
C27 C 0.1941(6) 0.0764(5) 1.2019(7) 0.053(3) Uani 1 1 d . . .
H27 H 0.2315 0.1124 1.2240 0.064 Uiso 1 1 calc R . .
C28 C 0.2104(5) 0.2039(5) 1.0687(7) 0.041(3) Uani 1 1 d . . .
C29 C 0.2118(5) 0.2330(6) 1.1367(7) 0.055(3) Uani 1 1 d . . .
H29 H 0.2282 0.2222 1.1791 0.066 Uiso 1 1 calc R . .
C30 C 0.1883(6) 0.2793(6) 1.1421(9) 0.065(4) Uani 1 1 d . . .
H30 H 0.1897 0.3000 1.1874 0.078 Uiso 1 1 calc R . .
C31 C 0.1640(8) 0.2924(7) 1.0801(11) 0.085(5) Uani 1 1 d . . .
H31 H 0.1481 0.3225 1.0833 0.102 Uiso 1 1 calc R . .
C32 C 0.1615(8) 0.2639(8) 1.0133(11) 0.102(5) Uani 1 1 d . . .
H32 H 0.1458 0.2753 0.9709 0.122 Uiso 1 1 calc R . .
C33 C 0.1828(7) 0.2175(7) 1.0091(7) 0.071(4) Uani 1 1 d . . .
H33 H 0.1780 0.1949 0.9642 0.085 Uiso 1 1 calc R . .
C34 C 0.3223(5) 0.1837(5) 1.1022(6) 0.038(3) Uani 1 1 d . . .
C35 C 0.3649(6) 0.2528(6) 1.0943(6) 0.051(3) Uani 1 1 d . . .
H35 H 0.3478 0.2789 1.0751 0.061 Uiso 1 1 calc R . .
C36 C 0.4298(6) 0.2824(6) 1.1139(7) 0.048(3) Uani 1 1 d . . .
H36 H 0.4577 0.3284 1.1064 0.058 Uiso 1 1 calc R . .
C37 C 0.4550(6) 0.2457(6) 1.1447(7) 0.058(3) Uani 1 1 d . . .
H37 H 0.4996 0.2671 1.1606 0.069 Uiso 1 1 calc R . .
C38 C 0.4152(6) 0.1767(6) 1.1528(7) 0.064(4) Uani 1 1 d . . .
H38 H 0.4331 0.1514 1.1722 0.076 Uiso 1 1 calc R . .
C39 C 0.3498(5) 0.1465(6) 1.1320(6) 0.043(3) Uani 1 1 d . . .
H39 H 0.3227 0.1002 1.1376 0.052 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 N1 90.3(3) . . ?
O1 Cu1 N2 91.4(3) . . ?
N1 Cu1 N2 156.7(3) . . ?
O1 Cu1 Cl1 164.4(5) . . ?
N1 Cu1 Cl1 92.1(3) . . ?
N2 Cu1 Cl1 92.5(3) . . ?
N4 P1 C34 113.7(4) . . ?
N4 P1 C22 108.0(5) . . ?
C34 P1 C22 109.4(5) . . ?
N4 P1 C28 110.3(5) . . ?
C34 P1 C28 108.0(5) . . ?
C22 P1 C28 107.2(5) . . ?
N4 P2 C10 112.5(5) . . ?
N4 P2 C4 108.2(5) . . ?
C10 P2 C4 108.9(5) . . ?
N4 P2 C16 112.8(5) . . ?
C10 P2 C16 107.5(5) . . ?
C4 P2 C16 106.8(5) . . ?
Cu1 O1 Cu1 119.91(5) 3_565 . ?
Cu1 O1 Cu1 119.91(5) 3_565 2_665 ?
Cu1 O1 Cu1 119.91(5) . 2_665 ?
C1 N1 N2 106.8(9) . 2_665 ?
C1 N1 Cu1 132.6(8) . . ?
N2 N1 Cu1 120.4(7) 2_665 . ?
C3 N2 N1 109.6(9) 3_565 3_565 ?
C3 N2 Cu1 132.8(8) 3_565 . ?
N1 N2 Cu1 117.1(6) 3_565 . ?
O3 N3 O2 123.8(11) . . ?
O3 N3 C2 120.8(12) . . ?
O2 N3 C2 115.3(12) . . ?
P2 N4 P1 139.1(5) . . ?
N1 C1 C2 109.1(10) . . ?
C1 C2 C3 106.4(9) . . ?
C1 C2 N3 128.1(12) . . ?
C3 C2 N3 125.5(12) . . ?
N2 C3 C2 108.1(10) 2_665 . ?
C5 C4 C9 117.7(11) . . ?
C5 C4 P2 122.2(9) . . ?
C9 C4 P2 120.1(9) . . ?
C6 C5 C4 121.5(12) . . ?
C5 C6 C7 119.8(13) . . ?
C8 C7 C6 120.6(13) . . ?
C7 C8 C9 117.6(13) . . ?
C8 C9 C4 122.8(12) . . ?
C11 C10 C15 118.7(11) . . ?
C11 C10 P2 117.7(9) . . ?
C15 C10 P2 123.4(9) . . ?
C10 C11 C12 122.4(12) . . ?
C13 C12 C11 119.3(13) . . ?
C12 C13 C14 120.4(12) . . ?
C13 C14 C15 119.8(13) . . ?
C10 C15 C14 119.3(12) . . ?
C17 C16 C21 118.1(10) . . ?
C17 C16 P2 120.8(8) . . ?
C21 C16 P2 121.0(9) . . ?
C16 C17 C18 121.2(11) . . ?
C17 C18 C19 118.2(12) . . ?
C20 C19 C18 120.6(12) . . ?
C21 C20 C19 120.3(12) . . ?
C20 C21 C16 121.4(12) . . ?
C27 C22 C23 119.5(11) . . ?
C27 C22 P1 123.1(9) . . ?
C23 C22 P1 117.2(9) . . ?
C24 C23 C22 119.4(13) . . ?
C23 C24 C25 121.1(13) . . ?
C26 C25 C24 118.7(13) . . ?
C25 C26 C27 120.9(13) . . ?
C26 C27 C22 120.3(12) . . ?
C33 C28 C29 118.7(11) . . ?
C33 C28 P1 123.4(10) . . ?
C29 C28 P1 117.7(9) . . ?
C28 C29 C30 119.9(11) . . ?
C31 C30 C29 118.2(13) . . ?
C30 C31 C32 122.8(14) . . ?
C31 C32 C33 118.6(15) . . ?
C28 C33 C32 121.6(13) . . ?
C35 C34 C39 117.4(10) . . ?
C35 C34 P1 120.8(9) . . ?
C39 C34 P1 121.5(8) . . ?
C36 C35 C34 121.5(11) . . ?
C35 C36 C37 120.2(12) . . ?
C36 C37 C38 120.7(11) . . ?
C39 C38 C37 119.1(11) . . ?
C38 C39 C34 121.1(11) . . ?
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 1.8890(13) . ?
Cu1 N1 1.955(8) . ?
Cu1 N2 1.969(9) . ?
Cu1 Cl1 2.279(3) . ?
P1 N4 1.584(9) . ?
P1 C34 1.776(11) . ?
P1 C22 1.784(11) . ?
P1 C28 1.797(11) . ?
P2 N4 1.559(8) . ?
P2 C10 1.757(11) . ?
P2 C4 1.769(11) . ?
P2 C16 1.822(10) . ?
O1 Cu1 1.8890(13) 3_565 ?
O1 Cu1 1.8890(13) 2_665 ?
O2 N3 1.253(13) . ?
O3 N3 1.181(12) . ?
N1 C1 1.352(12) . ?
N1 N2 1.380(11) 2_665 ?
N2 C3 1.320(12) 3_565 ?
N2 N1 1.380(11) 3_565 ?
N3 C2 1.401(13) . ?
C1 C2 1.368(14) . ?
C2 C3 1.396(14) . ?
C3 N2 1.320(12) 2_665 ?
C4 C5 1.355(14) . ?
C4 C9 1.387(14) . ?
C5 C6 1.354(16) . ?
C6 C7 1.405(18) . ?
C7 C8 1.351(17) . ?
C8 C9 1.382(16) . ?
C10 C11 1.349(14) . ?
C10 C15 1.360(15) . ?
C11 C12 1.385(15) . ?
C12 C13 1.307(16) . ?
C13 C14 1.388(17) . ?
C14 C15 1.392(16) . ?
C16 C17 1.345(13) . ?
C16 C21 1.392(13) . ?
C17 C18 1.367(15) . ?
C18 C19 1.382(16) . ?
C19 C20 1.343(16) . ?
C20 C21 1.315(15) . ?
C22 C27 1.366(14) . ?
C22 C23 1.389(15) . ?
C23 C24 1.340(16) . ?
C24 C25 1.396(18) . ?
C25 C26 1.349(17) . ?
C26 C27 1.358(15) . ?
C28 C33 1.350(15) . ?
C28 C29 1.377(14) . ?
C29 C30 1.414(15) . ?
C30 C31 1.339(17) . ?
C31 C32 1.345(19) . ?
C32 C33 1.379(17) . ?
C34 C35 1.392(14) . ?
C34 C39 1.394(13) . ?
C35 C36 1.339(15) . ?
C36 C37 1.353(15) . ?
C37 C38 1.384(15) . ?
C38 C39 1.352(14) . ?
