#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:55:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179353 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/50/4325026.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_4325026
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                102.958(4)
_cell_angle_beta                 99.504(4)
_cell_angle_gamma                100.302(4)
_cell_formula_units_Z            1
_cell_length_a                   7.0884(13)
_cell_length_b                   11.475(2)
_cell_length_c                   12.945(2)
_cell_measurement_reflns_used    1624
_cell_measurement_temperature    305(1)
_cell_measurement_theta_max      23.06
_cell_measurement_theta_min      2.80
_cell_volume                     986.2(3)
_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      305(1)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3824
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       prizm
_exptl_crystal_F_000             485
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0495
_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)+(0.0767P)²+0.5529P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                2402
_reflns_number_total             2765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1022483_si_001_05.cif
_cod_data_source_block           CuL_305
_cod_database_code               4325026
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 0.0435(3) Uani 1 2 d S
O2 O 0.1669(4) -0.1366(2) 0.0551(2) 0.0605(7) Uani 1 1 d .
N4 N 0.2915(4) -0.0584(3) -0.2529(2) 0.0437(7) Uani 1 1 d .
F4 F 0.2244(4) -0.4292(2) -0.0371(2) 0.0814(8) Uani 1 1 d .
N3 N 0.0976(4) -0.0327(3) -0.1376(2) 0.0446(8) Uani 1 1 d .
O02 O 0.2659(4) -0.3041(3) -0.4317(2) 0.0690(8) Uani 1 1 d .
O01 O -0.2232(4) -0.0927(3) -0.4713(2) 0.0688(8) Uani 1 1 d .
N1 N -0.1094(4) -0.1655(3) -0.4921(2) 0.0455(8) Uani 1 1 d .
C08 C 0.1011(5) -0.1109(3) -0.3100(3) 0.0417(8) Uani 1 1 d .
F5 F 0.4268(4) -0.2724(3) 0.0656(3) 0.1108(12) Uani 1 1 d .
F6 F 0.2006(6) -0.3686(3) 0.1242(2) 0.1123(13) Uani 1 1 d .
N2 N 0.1253(4) -0.2631(3) -0.4741(2) 0.0480(8) Uani 1 1 d .
C010 C 0.2808(6) -0.0131(3) -0.1509(3) 0.0483(9) Uani 1 1 d .
H01A H 0.3891 0.0277 -0.0953 0.058 Uiso 1 1 calc R
C07 C 0.0448(5) -0.1760(3) -0.4238(3) 0.0405(8) Uani 1 1 d .
C4 C 0.1041(6) -0.2462(4) 0.0119(3) 0.0523(10) Uani 1 1 d .
C01 C -0.1597(6) -0.2695(4) -0.5932(3) 0.0553(10) Uani 1 1 d .
C09 C -0.0135(5) -0.0924(3) -0.2383(3) 0.0452(9) Uani 1 1 d .
H09A H -0.1497 -0.1168 -0.2548 0.054 Uiso 1 1 calc R
C5 C 0.2416(7) -0.3290(4) 0.0405(4) 0.0648(12) Uani 1 1 d .
C3 C -0.0741(6) -0.3057(4) -0.0581(3) 0.0607(11) Uani 1 1 d .
H3A H -0.0950 -0.3902 -0.0855 0.073 Uiso 1 1 calc R
C06 C 0.1729(8) -0.2156(5) -0.6405(4) 0.0818(15) Uani 1 1 d .
H06A H 0.2964 -0.2392 -0.6385 0.123 Uiso 1 1 calc R
H06B H 0.1941 -0.1324 -0.5982 0.123 Uiso 1 1 calc R
H06C H 0.1123 -0.2221 -0.7142 0.123 Uiso 1 1 calc R
C011 C 0.4682(6) -0.0453(4) -0.2974(4) 0.0642(12) Uani 1 1 d .
H01B H 0.5805 -0.0054 -0.2396 0.096 Uiso 1 1 calc R
H01C H 0.4568 0.0031 -0.3487 0.096 Uiso 1 1 calc R
H01D H 0.4833 -0.1249 -0.3329 0.096 Uiso 1 1 calc R
C04 C 0.0401(6) -0.2993(4) -0.5941(3) 0.0512(10) Uani 1 1 d .
C05 C 0.0378(8) -0.4330(4) -0.6416(4) 0.0740(13) Uani 1 1 d .
H05A H -0.0466 -0.4836 -0.6102 0.111 Uiso 1 1 calc R
H05B H 0.1685 -0.4459 -0.6259 0.111 Uiso 1 1 calc R
H05C H -0.0099 -0.4542 -0.7188 0.111 Uiso 1 1 calc R
C03 C -0.3101(7) -0.3694(4) -0.5707(4) 0.0776(14) Uani 1 1 d .
H03A H -0.2512 -0.3947 -0.5097 0.116 Uiso 1 1 calc R
H03B H -0.3516 -0.4385 -0.6333 0.116 Uiso 1 1 calc R
H03C H -0.4215 -0.3375 -0.5552 0.116 Uiso 1 1 calc R
C02 C -0.2488(9) -0.2274(5) -0.6898(4) 0.0886(17) Uani 1 1 d .
H02A H -0.1525 -0.1651 -0.7027 0.133 Uiso 1 1 calc R
H02B H -0.3598 -0.1946 -0.6747 0.133 Uiso 1 1 calc R
H02C H -0.2904 -0.2958 -0.7530 0.133 Uiso 1 1 calc R
O1 O -0.2307(4) -0.1400(2) -0.0679(2) 0.0516(7) Uani 1 1 d .
F1 F -0.4486(4) -0.4442(2) -0.1588(3) 0.0930(9) Uani 1 1 d .
F2 F -0.5598(4) -0.2886(3) -0.1712(3) 0.0908(9) Uani 1 1 d .
F3 F -0.3708(5) -0.3448(3) -0.2727(2) 0.1088(12) Uani 1 1 d .
C2 C -0.4034(7) -0.3335(4) -0.1734(4) 0.0647(12) Uani 1 1 d .
C1 C -0.2225(6) -0.2510(4) -0.0905(3) 0.0514(10) 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'
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 180.0 2 .
O1 Cu N3 89.58(11) 2 2
O1 Cu N3 90.42(11) . 2
O1 Cu N3 90.42(11) 2 .
O1 Cu N3 89.58(11) . .
N3 Cu N3 180.0 2 .
O1 Cu O2 91.88(10) 2 .
O1 Cu O2 88.12(10) . .
N3 Cu O2 91.39(11) 2 .
N3 Cu O2 88.61(11) . .
O1 Cu O2 88.12(10) 2 2
O1 Cu O2 91.88(10) . 2
N3 Cu O2 88.61(11) 2 2
N3 Cu O2 91.39(11) . 2
O2 Cu O2 180.0 . 2
C4 O2 Cu 118.9(3) . .
C010 N4 C08 106.5(3) . .
C010 N4 C011 126.4(3) . .
C08 N4 C011 126.9(3) . .
C010 N3 C09 104.9(3) . .
C010 N3 Cu 128.8(2) . .
C09 N3 Cu 126.0(2) . .
O01 N1 C07 126.6(3) . .
O01 N1 C01 122.1(3) . .
C07 N1 C01 110.2(3) . .
C09 C08 N4 106.1(3) . .
C09 C08 C07 128.6(3) . .
N4 C08 C07 125.3(3) . .
O02 N2 C07 126.8(3) . .
O02 N2 C04 122.8(3) . .
C07 N2 C04 110.1(3) . .
N3 C010 N4 112.0(3) . .
N1 C07 N2 109.4(3) . .
N1 C07 C08 124.1(3) . .
N2 C07 C08 126.1(3) . .
O2 C4 C3 128.9(4) . .
O2 C4 C5 115.2(4) . .
C3 C4 C5 115.8(4) . .
N1 C01 C04 100.1(3) . .
N1 C01 C02 109.9(3) . .
C04 C01 C02 116.0(4) . .
N1 C01 C03 104.9(3) . .
C04 C01 C03 114.0(4) . .
C02 C01 C03 110.7(4) . .
C08 C09 N3 110.4(3) . .
F5 C5 F4 106.7(4) . .
F5 C5 F6 107.8(4) . .
F4 C5 F6 105.0(4) . .
F5 C5 C4 112.7(4) . .
F4 C5 C4 114.2(4) . .
F6 C5 C4 109.9(4) . .
C1 C3 C4 125.8(4) . .
N2 C04 C06 105.3(3) . .
N2 C04 C05 110.0(3) . .
C06 C04 C05 111.4(4) . .
N2 C04 C01 99.7(3) . .
C06 C04 C01 113.7(4) . .
C05 C04 C01 115.5(4) . .
C1 O1 Cu 124.7(3) . .
F2 C2 F1 106.7(4) . .
F2 C2 F3 106.6(4) . .
F1 C2 F3 108.1(4) . .
F2 C2 C1 112.8(4) . .
F1 C2 C1 112.8(4) . .
F3 C2 C1 109.5(4) . .
O1 C1 C3 130.1(4) . .
O1 C1 C2 112.7(4) . .
C3 C1 C2 117.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O1 1.995(2) 2
Cu O1 1.995(2) .
Cu N3 1.998(3) 2
Cu N3 1.998(3) .
Cu O2 2.292(3) .
Cu O2 2.292(3) 2
O2 C4 1.223(4) .
N4 C010 1.327(5) .
N4 C08 1.382(4) .
N4 C011 1.460(5) .
F4 C5 1.317(5) .
N3 C010 1.324(5) .
N3 C09 1.362(4) .
O02 N2 1.272(4) .
O01 N1 1.278(4) .
N1 C07 1.329(4) .
N1 C01 1.503(4) .
C08 C09 1.338(5) .
C08 C07 1.446(5) .
F5 C5 1.308(5) .
F6 C5 1.320(5) .
N2 C07 1.336(4) .
N2 C04 1.504(5) .
C4 C3 1.385(5) .
C4 C5 1.536(6) .
C01 C04 1.517(6) .
C01 C02 1.522(6) .
C01 C03 1.533(6) .
C3 C1 1.373(6) .
C06 C04 1.514(6) .
C04 C05 1.515(6) .
O1 C1 1.256(5) .
F1 C2 1.317(5) .
F2 C2 1.305(5) .
F3 C2 1.325(5) .
C2 C1 1.532(6) .
