#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305545.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_4305545
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-Br-pz)3Cl3]Cl(H2O)
_chemical_formula_sum            'C117 H98 Br3 Cl4 Cu3 N9 O2 P6'
_chemical_formula_weight         2420.01
_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                   22.8567(16)
_cell_length_b                   22.8567(16)
_cell_length_c                   18.0751(17)
_cell_measurement_temperature    293(2)
_cell_volume                     8177.8(11)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12097
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.921
_exptl_absorpt_correction_T_max  0.6803
_exptl_absorpt_correction_T_min  0.5922
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3687
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.029(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4860
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0292
_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)+(0.0614P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                4371
_reflns_number_total             4860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800531y-file001_1.cif
_cod_data_source_block           4
_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               4305545
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 0.90986(3) 0.92757(3) 0.29445(3) 0.04351(16) Uani 1 1 d . . .
Br1 Br 0.75595(3) 1.05838(4) 0.38845(3) 0.0721(2) Uani 1 1 d . . .
Cl1 Cl 0.80336(7) 0.84437(8) 0.26272(11) 0.0789(5) Uani 1 1 d . . .
Cl4 Cl 0.6667 0.3333 0.1313(3) 0.1434(17) Uani 1 3 d S . .
P1 P 0.78252(6) 0.61500(6) 0.13909(7) 0.0408(3) Uani 1 1 d . . .
P2 P 0.81059(6) 0.57292(6) -0.00466(7) 0.0397(3) Uani 1 1 d . . .
O1 O 1.0000 1.0000 0.2835(4) 0.0577(17) Uani 1 3 d S . .
N1 N 0.87902(19) 0.9909(2) 0.3181(2) 0.0456(10) Uani 1 1 d . . .
N2 N 0.94142(19) 0.86406(19) 0.3145(2) 0.0445(10) Uani 1 1 d . . .
N3 N 0.7813(2) 0.5671(2) 0.0758(2) 0.0511(11) Uani 1 1 d . . .
C1 C 0.8196(3) 0.9817(3) 0.3429(3) 0.0525(13) Uani 1 1 d . . .
H1 H 0.7809 0.9401 0.3506 0.063 Uiso 1 1 calc R . .
C2 C 0.8255(3) 1.0429(3) 0.3546(3) 0.0482(13) Uani 1 1 d . . .
C3 C 0.9090(3) 0.7992(2) 0.3355(3) 0.0482(13) Uani 1 1 d . . .
H3 H 0.8625 0.7706 0.3369 0.058 Uiso 1 1 calc R . .
C4 C 0.7195(2) 0.6394(2) 0.1258(3) 0.0466(12) Uani 1 1 d . . .
C5 C 0.6749(3) 0.6142(3) 0.0673(3) 0.0599(14) Uani 1 1 d . . .
H5 H 0.6770 0.5839 0.0346 0.072 Uiso 1 1 calc R . .
C6 C 0.6273(3) 0.6336(3) 0.0570(4) 0.0762(19) Uani 1 1 d . . .
H6 H 0.5976 0.6166 0.0171 0.091 Uiso 1 1 calc R . .
C7 C 0.6234(3) 0.6776(4) 0.1049(4) 0.0768(19) Uani 1 1 d . . .
H7 H 0.5908 0.6901 0.0981 0.092 Uiso 1 1 calc R . .
C8 C 0.6677(3) 0.7035(4) 0.1632(4) 0.0776(19) Uani 1 1 d . . .
H8 H 0.6655 0.7341 0.1953 0.093 Uiso 1 1 calc R . .
C9 C 0.7148(3) 0.6844(3) 0.1741(3) 0.0641(16) Uani 1 1 d . . .
H9 H 0.7442 0.7016 0.2142 0.077 Uiso 1 1 calc R . .
C10 C 0.7625(2) 0.5678(3) 0.2237(3) 0.0451(12) Uani 1 1 d . . .
C11 C 0.7351(3) 0.4982(3) 0.2215(4) 0.0566(14) Uani 1 1 d . . .
H11 H 0.7299 0.4765 0.1764 0.068 Uiso 1 1 calc R . .
C12 C 0.7157(3) 0.4613(3) 0.2861(4) 0.0657(16) Uani 1 1 d . . .
H12 H 0.6973 0.4147 0.2843 0.079 Uiso 1 1 calc R . .
C13 C 0.7231(3) 0.4923(4) 0.3527(4) 0.084(2) Uani 1 1 d . . .
H13 H 0.7098 0.4669 0.3960 0.101 Uiso 1 1 calc R . .
C14 C 0.7505(3) 0.5616(4) 0.3557(3) 0.0774(19) Uani 1 1 d . . .
H14 H 0.7555 0.5827 0.4011 0.093 Uiso 1 1 calc R . .
C15 C 0.7704(3) 0.5996(3) 0.2918(3) 0.0616(15) Uani 1 1 d . . .
H15 H 0.7889 0.6462 0.2942 0.074 Uiso 1 1 calc R . .
C16 C 0.8628(2) 0.6909(2) 0.1500(3) 0.0425(11) Uani 1 1 d . . .
C17 C 0.8747(3) 0.7538(3) 0.1258(3) 0.0570(14) Uani 1 1 d . . .
H17 H 0.8394 0.7586 0.1070 0.068 Uiso 1 1 calc R . .
C18 C 0.9388(3) 0.8089(3) 0.1297(4) 0.0708(18) Uani 1 1 d . . .
H18 H 0.9469 0.8508 0.1130 0.085 Uiso 1 1 calc R . .
C19 C 0.9912(3) 0.8023(3) 0.1581(3) 0.0718(18) Uani 1 1 d . . .
H19 H 1.0343 0.8398 0.1616 0.086 Uiso 1 1 calc R . .
C20 C 0.9796(3) 0.7406(4) 0.1813(3) 0.0679(17) Uani 1 1 d . . .
H20 H 1.0151 0.7362 0.1999 0.081 Uiso 1 1 calc R . .
C21 C 0.9158(3) 0.6848(3) 0.1774(3) 0.0536(14) Uani 1 1 d . . .
H21 H 0.9084 0.6430 0.1933 0.064 Uiso 1 1 calc R . .
C22 C 0.8719(2) 0.5461(2) -0.0060(3) 0.0459(12) Uani 1 1 d . . .
C23 C 0.9004(3) 0.5420(3) -0.0722(3) 0.0598(15) Uani 1 1 d . . .
H23 H 0.8877 0.5537 -0.1162 0.072 Uiso 1 1 calc R . .
C24 C 0.9473(3) 0.5209(3) -0.0735(4) 0.0724(18) Uani 1 1 d . . .
H24 H 0.9654 0.5174 -0.1183 0.087 Uiso 1 1 calc R . .
C25 C 0.9668(4) 0.5051(4) -0.0098(5) 0.089(2) Uani 1 1 d . . .
H25 H 1.0011 0.4944 -0.0103 0.107 Uiso 1 1 calc R . .
C26 C 0.9373(5) 0.5048(5) 0.0544(5) 0.110(3) Uani 1 1 d . . .
H26 H 0.9490 0.4909 0.0974 0.132 Uiso 1 1 calc R . .
C27 C 0.8892(4) 0.5251(4) 0.0573(4) 0.087(2) Uani 1 1 d . . .
H27 H 0.8688 0.5244 0.1021 0.104 Uiso 1 1 calc R . .
C28 C 0.7425(2) 0.5166(2) -0.0645(3) 0.0441(12) Uani 1 1 d . . .
C29 C 0.7449(3) 0.5261(3) -0.1400(3) 0.0574(14) Uani 1 1 d . . .
H29 H 0.7808 0.5642 -0.1613 0.069 Uiso 1 1 calc R . .
C30 C 0.6934(4) 0.4782(4) -0.1843(4) 0.0752(18) Uani 1 1 d . . .
H30 H 0.6949 0.4840 -0.2353 0.090 Uiso 1 1 calc R . .
C31 C 0.6405(3) 0.4225(3) -0.1524(5) 0.083(2) Uani 1 1 d . . .
H31 H 0.6060 0.3906 -0.1821 0.099 Uiso 1 1 calc R . .
C32 C 0.6378(3) 0.4132(3) -0.0780(5) 0.0787(19) Uani 1 1 d . . .
H32 H 0.6016 0.3751 -0.0570 0.094 Uiso 1 1 calc R . .
C33 C 0.6890(3) 0.4606(3) -0.0331(4) 0.0605(15) Uani 1 1 d . . .
H33 H 0.6871 0.4544 0.0179 0.073 Uiso 1 1 calc R . .
C34 C 0.8508(2) 0.6571(2) -0.0433(3) 0.0401(11) Uani 1 1 d . . .
C35 C 0.9209(2) 0.6990(2) -0.0370(3) 0.0471(12) Uani 1 1 d . . .
H35 H 0.9473 0.6818 -0.0189 0.057 Uiso 1 1 calc R . .
C36 C 0.9503(3) 0.7657(3) -0.0578(3) 0.0551(14) Uani 1 1 d . . .
H36 H 0.9968 0.7936 -0.0531 0.066 Uiso 1 1 calc R . .
C37 C 0.9126(3) 0.7913(3) -0.0851(3) 0.0639(16) Uani 1 1 d . . .
H37 H 0.9332 0.8365 -0.0990 0.077 Uiso 1 1 calc R . .
C38 C 0.8431(3) 0.7502(3) -0.0923(4) 0.0657(16) Uani 1 1 d . . .
H38 H 0.8171 0.7673 -0.1118 0.079 Uiso 1 1 calc R . .
C39 C 0.8132(3) 0.6836(3) -0.0701(3) 0.0521(13) Uani 1 1 d . . .
H39 H 0.7666 0.6563 -0.0734 0.063 Uiso 1 1 calc R . .
O2 O 0.0000 0.0000 0.1336(8) 0.142(4) Uani 1 3 d S . .
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'
Br Br -0.2901 2.4595 '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 90.74(13) . . ?
O1 Cu1 N2 91.40(12) . . ?
N1 Cu1 N2 156.65(18) . . ?
O1 Cu1 Cl1 159.5(2) . . ?
N1 Cu1 Cl1 92.46(12) . . ?
N2 Cu1 Cl1 93.64(12) . . ?
N3 P1 C10 106.9(2) . . ?
N3 P1 C16 114.0(2) . . ?
C10 P1 C16 108.5(2) . . ?
N3 P1 C4 112.3(2) . . ?
C10 P1 C4 107.2(2) . . ?
C16 P1 C4 107.7(2) . . ?
N3 P2 C22 110.8(2) . . ?
N3 P2 C28 108.3(2) . . ?
C22 P2 C28 107.0(2) . . ?
N3 P2 C34 114.5(2) . . ?
C22 P2 C34 106.9(2) . . ?
C28 P2 C34 109.1(2) . . ?
Cu1 O1 Cu1 118.92(7) 3_675 2_765 ?
Cu1 O1 Cu1 118.92(7) 3_675 . ?
Cu1 O1 Cu1 118.92(7) 2_765 . ?
C1 N1 N2 107.7(4) . 3_675 ?
C1 N1 Cu1 132.0(4) . . ?
N2 N1 Cu1 120.2(3) 3_675 . ?
C3 N2 N1 108.7(4) . 2_765 ?
C3 N2 Cu1 132.2(3) . . ?
N1 N2 Cu1 118.5(3) 2_765 . ?
P1 N3 P2 138.7(3) . . ?
N1 C1 C2 108.6(5) . . ?
C1 C2 C3 107.3(4) . 3_675 ?
C1 C2 Br1 125.8(4) . . ?
C3 C2 Br1 126.9(4) 3_675 . ?
N2 C3 C2 107.6(5) . 2_765 ?
C5 C4 C9 118.4(5) . . ?
C5 C4 P1 120.8(4) . . ?
C9 C4 P1 120.9(4) . . ?
C6 C5 C4 120.6(6) . . ?
C7 C6 C5 120.2(6) . . ?
C6 C7 C8 119.9(6) . . ?
C9 C8 C7 120.3(7) . . ?
C8 C9 C4 120.6(6) . . ?
C11 C10 C15 119.2(5) . . ?
C11 C10 P1 119.9(4) . . ?
C15 C10 P1 120.8(4) . . ?
C12 C11 C10 120.0(6) . . ?
C13 C12 C11 120.8(6) . . ?
C12 C13 C14 119.8(6) . . ?
C15 C14 C13 120.5(7) . . ?
C14 C15 C10 119.7(6) . . ?
C21 C16 C17 119.3(5) . . ?
C21 C16 P1 117.7(4) . . ?
C17 C16 P1 122.7(4) . . ?
C18 C17 C16 119.9(5) . . ?
C19 C18 C17 120.3(6) . . ?
C20 C19 C18 119.8(6) . . ?
C19 C20 C21 120.7(6) . . ?
C20 C21 C16 120.1(6) . . ?
C27 C22 C23 117.9(5) . . ?
C27 C22 P2 121.4(5) . . ?
C23 C22 P2 120.6(4) . . ?
C24 C23 C22 120.7(6) . . ?
C25 C24 C23 119.9(6) . . ?
C26 C25 C24 120.5(6) . . ?
C25 C26 C27 120.8(7) . . ?
C22 C27 C26 119.9(7) . . ?
C29 C28 C33 120.1(5) . . ?
C29 C28 P2 122.0(4) . . ?
C33 C28 P2 117.8(4) . . ?
C28 C29 C30 119.6(6) . . ?
C31 C30 C29 119.7(7) . . ?
C32 C31 C30 120.8(6) . . ?
C31 C32 C33 120.1(6) . . ?
C28 C33 C32 119.7(6) . . ?
C39 C34 C35 119.0(5) . . ?
C39 C34 P2 120.8(4) . . ?
C35 C34 P2 119.7(4) . . ?
C36 C35 C34 119.6(5) . . ?
C37 C36 C35 120.9(5) . . ?
C36 C37 C38 120.1(5) . . ?
C39 C38 C37 119.2(5) . . ?
C34 C39 C38 121.2(5) . . ?
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 1.9012(10) . ?
Cu1 N1 1.949(4) . ?
Cu1 N2 1.951(4) . ?
Cu1 Cl1 2.2894(15) . ?
Br1 C2 1.894(5) . ?
P1 N3 1.574(4) . ?
P1 C10 1.793(5) . ?
P1 C16 1.798(5) . ?
P1 C4 1.803(5) . ?
P2 N3 1.579(4) . ?
P2 C22 1.789(5) . ?
P2 C28 1.801(5) . ?
P2 C34 1.808(5) . ?
O1 Cu1 1.9012(9) 3_675 ?
O1 Cu1 1.9012(9) 2_765 ?
N1 C1 1.342(6) . ?
N1 N2 1.359(5) 3_675 ?
N2 C3 1.339(6) . ?
N2 N1 1.359(5) 2_765 ?
C1 C2 1.355(7) . ?
C2 C3 1.374(7) 3_675 ?
C3 C2 1.374(7) 2_765 ?
C4 C5 1.379(7) . ?
C4 C9 1.393(7) . ?
C5 C6 1.377(8) . ?
C6 C7 1.363(9) . ?
C7 C8 1.373(10) . ?
C8 C9 1.363(8) . ?
C10 C11 1.388(7) . ?
C10 C15 1.395(8) . ?
C11 C12 1.378(8) . ?
C12 C13 1.364(10) . ?
C13 C14 1.383(10) . ?
C14 C15 1.377(8) . ?
C16 C21 1.379(7) . ?
C16 C17 1.393(7) . ?
C17 C18 1.376(8) . ?
C18 C19 1.379(10) . ?
C19 C20 1.363(10) . ?
C20 C21 1.378(8) . ?
C22 C27 1.374(8) . ?
C22 C23 1.388(7) . ?
C23 C24 1.379(8) . ?
C24 C25 1.349(10) . ?
C25 C26 1.340(11) . ?
C26 C27 1.389(10) . ?
C28 C29 1.380(8) . ?
C28 C33 1.376(7) . ?
C29 C30 1.391(8) . ?
C30 C31 1.370(10) . ?
C31 C32 1.358(10) . ?
C32 C33 1.391(8) . ?
C34 C39 1.363(7) . ?
C34 C35 1.400(7) . ?
C35 C36 1.376(7) . ?
C36 C37 1.355(8) . ?
C37 C38 1.388(8) . ?
C38 C39 1.380(7) . ?
