#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:55:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179353 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/50/4325024.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_4325024
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            'C32 H36 Cu F12 N8 O8'
_chemical_formula_weight         952.23
_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                101.781(5)
_cell_angle_beta                 99.593(5)
_cell_angle_gamma                100.640(6)
_cell_formula_units_Z            1
_cell_length_a                   6.9848(19)
_cell_length_b                   11.290(3)
_cell_length_c                   12.650(4)
_cell_measurement_reflns_used    1129
_cell_measurement_temperature    240(1)
_cell_measurement_theta_max      23.15
_cell_measurement_theta_min      2.21
_cell_volume                     937.9(5)
_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      240(1)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4042
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       prizm
_exptl_crystal_F_000             485
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0659
_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)+(0.0208P)²+7.8575P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1468
_reflns_number_gt                2077
_reflns_number_total             2655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1022483_si_001_03.cif
_cod_data_source_block           CuL_240
_cod_database_code               4325024
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 0.5000 0.5000 0.5000 0.0267(3) Uani 1 2 d S
O1 O 0.7319(6) 0.6390(4) 0.5665(3) 0.0325(11) Uani 1 1 d .
C1 C 0.9068(11) 0.8314(6) 0.6748(6) 0.0419(18) Uani 1 1 d .
F1 F 0.8733(7) 0.8422(5) 0.7749(4) 0.0740(15) Uani 1 1 d .
F2 F 1.0639(6) 0.7845(4) 0.6717(4) 0.0598(12) Uani 1 1 d .
F3 F 0.9539(6) 0.9437(4) 0.6599(4) 0.0621(13) Uani 1 1 d .
C2 C 0.7257(10) 0.7495(6) 0.5909(5) 0.0332(16) Uani 1 1 d .
C3 C 0.5767(10) 0.8068(6) 0.5603(6) 0.0402(17) Uani 1 1 d .
H3A H 0.5997 0.8919 0.5895 0.048 Uiso 1 1 calc R
C4 C 0.3939(9) 0.7490(6) 0.4896(5) 0.0324(15) Uani 1 1 d .
C5 C 0.2545(11) 0.8334(7) 0.4626(6) 0.0417(18) Uani 1 1 d .
F4 F 0.2922(8) 0.8715(4) 0.3744(4) 0.0659(14) Uani 1 1 d .
F5 F 0.0689(6) 0.7757(4) 0.4396(4) 0.0697(14) Uani 1 1 d .
F6 F 0.2805(6) 0.9325(4) 0.5408(3) 0.0541(11) Uani 1 1 d .
O2 O 0.3322(7) 0.6380(4) 0.4432(4) 0.0383(11) Uani 1 1 d .
O01 O 0.7291(7) 0.5919(5) 0.9767(4) 0.0450(13) Uani 1 1 d .
N1 N 0.6180(7) 0.6664(5) 0.9959(4) 0.0299(12) Uani 1 1 d .
C01 C 0.6699(10) 0.7707(6) 1.0963(5) 0.0348(16) Uani 1 1 d .
C02 C 0.7559(12) 0.7311(8) 1.1948(6) 0.056(2) Uani 1 1 d .
H02A H 0.8838 0.7143 1.1881 0.085 Uiso 1 1 calc R
H02B H 0.6686 0.6573 1.2003 0.085 Uiso 1 1 calc R
H02C H 0.7712 0.7960 1.2599 0.085 Uiso 1 1 calc R
C03 C 0.8169(10) 0.8707(7) 1.0709(6) 0.051(2) Uani 1 1 d .
H03A H 0.9420 0.8468 1.0719 0.077 Uiso 1 1 calc R
H03B H 0.8356 0.9470 1.1255 0.077 Uiso 1 1 calc R
H03C H 0.7669 0.8821 0.9992 0.077 Uiso 1 1 calc R
C04 C 0.4632(10) 0.8001(6) 1.0965(5) 0.0374(17) Uani 1 1 d .
C05 C 0.4648(11) 0.9312(7) 1.1429(6) 0.0479(19) Uani 1 1 d .
H05A H 0.3303 0.9407 1.1395 0.072 Uiso 1 1 calc R
H05B H 0.5288 0.9822 1.1010 0.072 Uiso 1 1 calc R
H05C H 0.5363 0.9560 1.2185 0.072 Uiso 1 1 calc R
C06 C 0.3338(12) 0.7134(8) 1.1462(6) 0.057(2) Uani 1 1 d .
H06A H 0.2070 0.7351 1.1447 0.085 Uiso 1 1 calc R
H06B H 0.3978 0.7205 1.2212 0.085 Uiso 1 1 calc R
H06C H 0.3144 0.6294 1.1042 0.085 Uiso 1 1 calc R
N2 N 0.3777(7) 0.7619(5) 0.9761(4) 0.0312(13) Uani 1 1 d .
O02 O 0.2368(7) 0.8041(4) 0.9322(4) 0.0446(12) Uani 1 1 d .
C07 C 0.4565(8) 0.6754(6) 0.9264(5) 0.0259(14) Uani 1 1 d .
C08 C 0.4010(8) 0.6106(6) 0.8138(5) 0.0272(14) Uani 1 1 d .
C09 C 0.5146(9) 0.5906(6) 0.7397(5) 0.0295(15) Uani 1 1 d .
H09A H 0.6530 0.6147 0.7557 0.035 Uiso 1 1 calc R
N3 N 0.4029(7) 0.5314(5) 0.6389(4) 0.0294(12) Uani 1 1 d .
C010 C 0.2185(9) 0.5113(6) 0.6535(5) 0.0302(15) Uani 1 1 d .
H01A H 0.1081 0.4690 0.5979 0.036 Uiso 1 1 calc R
N4 N 0.2087(7) 0.5576(5) 0.7549(4) 0.0286(12) Uani 1 1 d .
C011 C 0.0313(9) 0.5453(7) 0.8020(6) 0.0424(18) Uani 1 1 d .
H01E H -0.0842 0.5054 0.7442 0.064 Uiso 1 1 calc R
H01B H 0.0177 0.6261 0.8373 0.064 Uiso 1 1 calc R
H01C H 0.0435 0.4961 0.8553 0.064 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'
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'
F F 0.0171 0.0103 '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
O1 Cu O1 179.998(1) . 2_666
O1 Cu N3 89.66(18) . .
O1 Cu N3 90.34(18) 2_666 .
O1 Cu N3 90.34(18) . 2_666
O1 Cu N3 89.66(18) 2_666 2_666
N3 Cu N3 180.0(2) . 2_666
O1 Cu O2 91.76(17) . 2_666
O1 Cu O2 88.24(17) 2_666 2_666
N3 Cu O2 91.42(19) . 2_666
N3 Cu O2 88.58(19) 2_666 2_666
O1 Cu O2 88.24(17) . .
O1 Cu O2 91.76(17) 2_666 .
N3 Cu O2 88.58(19) . .
N3 Cu O2 91.42(19) 2_666 .
O2 Cu O2 180.00(12) 2_666 .
C2 O1 Cu 125.2(4) . .
F2 C1 F3 107.0(6) . .
F2 C1 F1 107.4(6) . .
F3 C1 F1 107.3(6) . .
F2 C1 C2 111.6(6) . .
F3 C1 C2 113.1(6) . .
F1 C1 C2 110.0(6) . .
O1 C2 C3 130.1(6) . .
O1 C2 C1 113.9(6) . .
C3 C2 C1 115.9(6) . .
C2 C3 C4 125.8(6) . .
O2 C4 C3 127.8(6) . .
O2 C4 C5 115.7(6) . .
C3 C4 C5 116.4(6) . .
F6 C5 F5 108.9(6) . .
F6 C5 F4 106.4(6) . .
F5 C5 F4 107.4(6) . .
F6 C5 C4 113.1(6) . .
F5 C5 C4 112.0(6) . .
F4 C5 C4 108.6(6) . .
C4 O2 Cu 118.5(4) . .
O01 N1 C07 126.8(5) . .
O01 N1 C01 122.4(5) . .
C07 N1 C01 110.3(5) . .
C02 C01 N1 111.0(6) . .
C02 C01 C03 111.8(6) . .
N1 C01 C03 105.1(5) . .
C02 C01 C04 114.7(6) . .
N1 C01 C04 99.6(5) . .
C03 C01 C04 113.6(6) . .
C05 C04 N2 111.6(6) . .
C05 C04 C06 111.8(6) . .
N2 C04 C06 105.3(6) . .
C05 C04 C01 115.3(6) . .
N2 C04 C01 99.5(5) . .
C06 C04 C01 112.3(6) . .
O02 N2 C07 126.4(5) . .
O02 N2 C04 122.1(5) . .
C07 N2 C04 111.3(5) . .
N2 C07 N1 109.2(5) . .
N2 C07 C08 127.0(6) . .
N1 C07 C08 123.3(5) . .
C09 C08 N4 104.5(5) . .
C09 C08 C07 129.7(5) . .
N4 C08 C07 125.8(5) . .
C08 C09 N3 111.3(5) . .
C010 N3 C09 104.6(5) . .
C010 N3 Cu 129.1(4) . .
C09 N3 Cu 126.0(4) . .
N4 C010 N3 112.1(5) . .
C010 N4 C08 107.5(5) . .
C010 N4 C011 126.9(5) . .
C08 N4 C011 125.3(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O1 1.965(4) .
Cu O1 1.965(4) 2_666
Cu N3 1.977(5) .
Cu N3 1.977(5) 2_666
Cu O2 2.274(4) 2_666
Cu O2 2.274(4) .
O1 C2 1.233(7) .
C1 F2 1.306(8) .
C1 F3 1.310(8) .
C1 F1 1.312(8) .
C1 C2 1.517(9) .
C2 C3 1.367(9) .
C3 C4 1.389(9) .
C4 O2 1.232(7) .
C4 C5 1.529(9) .
C5 F6 1.294(8) .
C5 F5 1.294(8) .
C5 F4 1.323(8) .
O01 N1 1.261(6) .
N1 C07 1.344(7) .
N1 C01 1.486(8) .
C01 C02 1.480(9) .
C01 C03 1.504(10) .
C01 C04 1.541(9) .
C04 C05 1.473(9) .
C04 N2 1.481(8) .
C04 C06 1.512(10) .
N2 O02 1.265(6) .
N2 C07 1.310(7) .
C07 C08 1.414(8) .
C08 C09 1.336(8) .
C08 N4 1.380(7) .
C09 N3 1.344(7) .
N3 C010 1.316(8) .
C010 N4 1.300(8) .
N4 C011 1.458(8) .
