#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:55:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179353 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/50/4325030.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_4325030
loop_
_publ_author_name
'Victor I. Ovcharenko'
'Sergei V. Fokin'
'Elena Yu. Fursova'
'Olga V. Kuznetsova'
'Eugene V. Tretyakov'
'Galina V. Romanenko'
'Artem S. Bogomyakov'
_publ_section_title
;
 "Jumping Crystals": Oxygen-Evolving Metal-Nitroxide Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4307
_journal_page_last               4312
_journal_paper_doi               10.1021/ic1022483
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C34 H56 Cl4 Cu N8 O8'
_chemical_formula_weight         910.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.302(2)
_cell_angle_beta                 112.182(2)
_cell_angle_gamma                92.859(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2351(11)
_cell_length_b                   10.8412(13)
_cell_length_c                   12.0491(15)
_cell_measurement_reflns_used    1588
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.05
_cell_measurement_theta_min      2.39
_cell_volume                     1113.4(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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8713
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       prizm
_exptl_crystal_F_000             477
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0508
_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)+(0.0556P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                2324
_reflns_number_total             3212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1022483_si_001_09.cif
_cod_data_source_block           CuL5
_cod_database_code               4325030
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cu Cu 0.0000 0.0000 0.0000 0.0321(2) Uani 1 2 d S
O1A O 0.0439(3) -0.1249(2) 0.1186(2) 0.0371(7) Uani 1 1 d .
O2A O 0.0398(4) 0.0450(3) 0.2238(3) 0.0595(9) Uani 1 1 d .
C1A C 0.0646(4) -0.0663(4) 0.2176(4) 0.0404(10) Uani 1 1 d .
C2A C 0.1256(5) -0.1363(4) 0.3332(4) 0.0465(11) Uani 1 1 d .
C3A C 0.2731(7) -0.0667(6) 0.4214(5) 0.097(2) Uani 1 1 d .
H28A H 0.2498 0.0153 0.4393 0.14(3) Uiso 1 1 calc R
H28B H 0.3512 -0.0617 0.3868 0.11(2) Uiso 1 1 calc R
H28C H 0.3119 -0.1095 0.4940 0.093(18) Uiso 1 1 calc R
C4A C 0.1648(10) -0.2672(5) 0.3070(5) 0.099(2) Uani 1 1 d .
H29A H 0.2000 -0.3098 0.3798 0.094(17) Uiso 1 1 calc R
H29B H 0.2460 -0.2624 0.2755 0.17(4) Uiso 1 1 calc R
H29C H 0.0729 -0.3114 0.2491 0.46(10) Uiso 1 1 calc R
C5A C 0.0009(9) -0.1436(9) 0.3843(7) 0.125(3) Uani 1 1 d .
H37A H -0.0214 -0.0615 0.4029 0.15(3) Uiso 1 1 calc R
H37B H 0.0367 -0.1878 0.4561 0.096(18) Uiso 1 1 calc R
H37C H -0.0924 -0.1861 0.3266 0.19(4) Uiso 1 1 calc R
O1 O 0.6863(3) 0.2431(3) 0.3386(2) 0.0521(8) Uani 1 1 d .
N1 N 0.6873(3) 0.2836(3) 0.2408(3) 0.0381(8) Uani 1 1 d .
C1 C 0.7917(4) 0.3943(4) 0.2395(4) 0.0412(10) Uani 1 1 d .
C2 C 0.7215(8) 0.5058(5) 0.2777(6) 0.0687(16) Uani 1 1 d .
H1AA H 0.733(5) 0.486(4) 0.369(4) 0.080(16) Uiso 1 1 d .
H1AB H 0.612(6) 0.519(4) 0.212(4) 0.086(18) Uiso 1 1 d .
H1AC H 0.786(5) 0.572(4) 0.283(4) 0.066(15) Uiso 1 1 d .
C3 C 0.9559(6) 0.3795(7) 0.3298(6) 0.0678(16) Uani 1 1 d .
H16A H 0.994(6) 0.299(5) 0.320(4) 0.09(2) Uiso 1 1 d .
H16B H 0.957(5) 0.387(5) 0.409(5) 0.085(19) Uiso 1 1 d .
H16C H 1.027(6) 0.441(4) 0.328(4) 0.081(17) Uiso 1 1 d .
C4 C 0.7717(4) 0.3883(3) 0.1056(3) 0.0365(10) Uani 1 1 d .
C5 C 0.7554(7) 0.5115(5) 0.0480(6) 0.0606(14) Uani 1 1 d .
H20A H 0.662(5) 0.557(4) 0.053(3) 0.060(14) Uiso 1 1 d .
H20B H 0.741(5) 0.495(4) -0.033(4) 0.066(16) Uiso 1 1 d .
H20C H 0.847(5) 0.557(5) 0.085(4) 0.084(17) Uiso 1 1 d .
C6 C 0.8948(6) 0.3158(6) 0.0806(6) 0.0573(14) Uani 1 1 d .
H19A H 0.917(5) 0.240(5) 0.126(4) 0.084(18) Uiso 1 1 d .
H19B H 0.990(5) 0.357(4) 0.107(4) 0.063(15) Uiso 1 1 d .
H19C H 0.869(4) 0.307(4) -0.001(4) 0.047(13) Uiso 1 1 d .
N2 N 0.6201(3) 0.3101(3) 0.0488(3) 0.0364(8) Uani 1 1 d .
O2 O 0.5449(3) 0.2979(3) -0.0649(2) 0.0496(8) Uani 1 1 d .
C7 C 0.5866(4) 0.2458(3) 0.1297(3) 0.0331(9) Uani 1 1 d .
C8 C 0.4608(4) 0.1502(3) 0.1045(3) 0.0331(9) Uani 1 1 d .
C9 C 0.3037(5) 0.1525(4) 0.0463(4) 0.0377(10) Uani 1 1 d .
H17A H 0.254(3) 0.210(3) 0.008(3) 0.010(9) Uiso 1 1 d .
N3 N 0.2304(3) 0.0420(3) 0.0513(3) 0.0354(8) Uani 1 1 d .
C10 C 0.3441(4) -0.0273(4) 0.1119(4) 0.0371(10) Uani 1 1 d .
H10A H 0.334(4) -0.108(3) 0.123(3) 0.028(10) Uiso 1 1 d .
N4 N 0.4854(3) 0.0334(3) 0.1458(3) 0.0360(8) Uani 1 1 d .
C11 C 0.6354(6) -0.0183(5) 0.2122(6) 0.0498(13) Uani 1 1 d .
H21A H 0.627(4) -0.099(4) 0.198(3) 0.042(13) Uiso 1 1 d .
H21B H 0.666(5) 0.007(4) 0.291(5) 0.078(18) Uiso 1 1 d .
H21C H 0.701(6) 0.009(5) 0.183(4) 0.08(2) Uiso 1 1 d .
C1X C 1.3503(8) 0.2676(6) 0.3647(6) 0.087(2) Uani 1 1 d .
H24A H 1.260(8) 0.225(7) 0.324(6) 0.16(3) Uiso 1 1 d .
H24B H 1.459(7) 0.241(5) 0.381(5) 0.12(2) Uiso 1 1 d .
Cl1 Cl 1.3551(2) 0.28782(18) 0.51040(16) 0.1171(7) Uani 1 1 d .
Cl2 Cl 1.34095(18) 0.40678(17) 0.29477(19) 0.1166(7) Uani 1 1 d .
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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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'
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
O1A Cu O1A 180.0 2 .
O1A Cu N3 89.58(11) 2 2
O1A Cu N3 90.42(11) . 2
O1A Cu N3 90.42(11) 2 .
O1A Cu N3 89.58(11) . .
N3 Cu N3 180.0 2 .
O1A Cu C1A 28.13(12) 2 2
O1A Cu C1A 151.87(12) . 2
N3 Cu C1A 86.14(12) 2 2
N3 Cu C1A 93.86(12) . 2
O1A Cu C1A 151.87(12) 2 .
O1A Cu C1A 28.13(12) . .
N3 Cu C1A 93.86(12) 2 .
N3 Cu C1A 86.14(12) . .
C1A Cu C1A 180.0 2 .
O1A Cu O2A 124.31(10) 2 .
O1A Cu O2A 55.69(10) . .
N3 Cu O2A 93.27(11) 2 .
N3 Cu O2A 86.73(11) . .
C1A Cu O2A 152.34(11) 2 .
C1A Cu O2A 27.66(10) . .
O1A Cu O2A 55.69(10) 2 2
O1A Cu O2A 124.31(10) . 2
N3 Cu O2A 86.73(11) 2 2
N3 Cu O2A 93.27(11) . 2
C1A Cu O2A 27.66(10) 2 2
C1A Cu O2A 152.34(11) . 2
O2A Cu O2A 180.00(3) . 2
C1A O1A Cu 105.5(2) . .
C1A O2A Cu 76.1(2) . .
O2A C1A O1A 122.3(4) . .
O2A C1A C2A 119.5(4) . .
O1A C1A C2A 118.2(4) . .
O2A C1A Cu 76.3(2) . .
O1A C1A Cu 46.35(18) . .
C2A C1A Cu 163.0(3) . .
C5A C2A C3A 110.6(6) . .
C5A C2A C1A 108.4(4) . .
C3A C2A C1A 108.8(4) . .
C5A C2A C4A 109.5(6) . .
C3A C2A C4A 108.7(5) . .
C1A C2A C4A 110.9(4) . .
O1 N1 C7 125.8(3) . .
O1 N1 C1 122.0(3) . .
C7 N1 C1 111.7(3) . .
N1 C1 C3 108.7(4) . .
N1 C1 C2 105.2(3) . .
C3 C1 C2 110.6(5) . .
N1 C1 C4 101.0(3) . .
C3 C1 C4 115.9(4) . .
C2 C1 C4 114.2(4) . .
N2 C4 C5 109.2(3) . .
N2 C4 C6 105.8(3) . .
C5 C4 C6 110.7(4) . .
N2 C4 C1 101.1(3) . .
C5 C4 C1 115.6(4) . .
C6 C4 C1 113.5(4) . .
O2 N2 C7 125.5(3) . .
O2 N2 C4 122.4(3) . .
C7 N2 C4 111.7(3) . .
N2 C7 N1 109.7(3) . .
N2 C7 C8 126.4(3) . .
N1 C7 C8 123.9(4) . .
C9 C8 N4 105.7(3) . .
C9 C8 C7 131.3(4) . .
N4 C8 C7 122.9(3) . .
N3 C9 C8 110.5(4) . .
N3 C9 Cu 31.46(17) . .
C8 C9 Cu 141.4(3) . .
C10 N3 C9 105.2(3) . .
C10 N3 Cu 126.5(3) . .
C9 N3 Cu 127.7(3) . .
N3 C10 N4 111.9(4) . .
N3 C10 Cu 32.62(17) . .
N4 C10 Cu 144.0(3) . .
C10 N4 C8 106.7(3) . .
C10 N4 C11 125.4(4) . .
C8 N4 C11 127.9(4) . .
Cl1 C1X Cl2 112.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O1A 1.952(2) 2
Cu O1A 1.952(2) .
Cu N3 2.001(3) 2
Cu N3 2.001(3) .
Cu C1A 2.600(4) 2
Cu C1A 2.600(4) .
Cu O2A 2.602(3) .
Cu O2A 2.602(3) 2
O1A C1A 1.272(5) .
O2A C1A 1.244(5) .
C1A C2A 1.539(5) .
C2A C5A 1.496(7) .
C2A C3A 1.515(6) .
C2A C4A 1.532(7) .
O1 N1 1.277(4) .
N1 C7 1.342(5) .
N1 C1 1.505(5) .
C1 C3 1.517(6) .
C1 C2 1.534(6) .
C1 C4 1.551(5) .
C4 N2 1.503(4) .
C4 C5 1.518(6) .
C4 C6 1.526(6) .
N2 O2 1.278(4) .
N2 C7 1.338(5) .
C7 C8 1.451(5) .
C8 C9 1.354(5) .
C8 N4 1.378(4) .
C9 N3 1.361(5) .
N3 C10 1.321(5) .
C10 N4 1.339(5) .
N4 C11 1.466(5) .
C1X Cl1 1.744(7) .
C1X Cl2 1.748(7) .
