#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:57:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179355 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/52/4325223.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_4325223
loop_
_publ_author_name
'Martha Baskett'
'Armando Paduan-Filho'
'Nei Fernandes Oliveira'
'A. Chandrasekaran'
'Joel T. Mague'
'Paul M. Lahti'
_publ_contact_author_email       'lahti@chem.umass.edu '
_publ_contact_author_fax         '1-413-545-4490 '
_publ_contact_author_phone       '1-413-545-4890 '
_publ_section_title
;
 Loops, Chains, Sheets, and Networks from Variable Coordination of
 Cu(hfac)2 with a Flexibly Hinged Aminoxyl Radical Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5060
_journal_page_last               5074
_journal_paper_doi               10.1021/ic200362c
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C58 H38 Cu3 F36 N6 O14'
_chemical_formula_weight         1917.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 92.6405(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.9104(2)
_cell_length_b                   11.68780(10)
_cell_length_c                   20.5148(2)
_cell_measurement_reflns_used    5880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      4.08
_cell_volume                     3571.31(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10546
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.18
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             1902
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         6208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0499
_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)+(0.0334P)²+20.7809P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1422
_reflns_number_gt                5499
_reflns_number_total             6208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200362c_si_002_07.cif
_cod_data_source_block           mb320_100K
_cod_database_code               4325223
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Cu1 Cu 0.39056(3) -0.01280(5) 0.20912(2) 0.01755(16) Uani 1 1 d .
Cu2 Cu 0.0000 0.5000 0.0000 0.01643(19) Uani 1 2 d S
O1 O 0.2575(2) 0.0910(3) 0.20726(14) 0.0216(7) Uani 1 1 d .
O2 O 0.3987(2) 0.0347(3) 0.11835(14) 0.0211(7) Uani 1 1 d .
O3 O 0.3117(2) -0.1407(3) 0.17761(15) 0.0219(7) Uani 1 1 d .
O4 O 0.5039(2) -0.1394(3) 0.20294(16) 0.0256(7) Uani 1 1 d .
O5 O -0.0384(2) 0.6311(3) 0.05111(14) 0.0204(7) Uani 1 1 d .
O6 O 0.0880(2) 0.5903(3) -0.04509(15) 0.0205(7) Uani 1 1 d .
O7 O 0.46061(19) 0.1181(3) 0.24280(14) 0.0181(6) Uani 1 1 d .
N1 N 0.1403(2) 0.4504(3) 0.19876(17) 0.0178(8) Uani 1 1 d .
N2 N 0.5169(2) 0.1706(3) 0.20662(17) 0.0190(8) Uani 1 1 d .
N3 N 0.1081(2) 0.4423(3) 0.08496(18) 0.0196(8) Uani 1 1 d .
C1 C 0.1099(3) 0.0937(4) 0.1629(2) 0.0265(11) Uani 1 1 d .
C2 C 0.2120(3) 0.0860(4) 0.1555(2) 0.0201(10) Uani 1 1 d .
C3 C 0.2432(3) 0.0751(4) 0.0917(2) 0.0220(10) Uani 1 1 d .
H3 H 0.2015 0.0851 0.0557 0.026 Uiso 1 1 calc R
C4 C 0.3315(3) 0.0505(4) 0.0792(2) 0.0208(10) Uani 1 1 d .
C5 C 0.3553(3) 0.0348(5) 0.0083(2) 0.0270(11) Uani 1 1 d .
C6 C 0.2551(3) -0.2754(4) 0.1041(2) 0.0294(11) Uani 1 1 d .
C7 C 0.3350(3) -0.2241(4) 0.1434(2) 0.0225(10) Uani 1 1 d .
C8 C 0.4191(3) -0.2720(4) 0.1366(2) 0.0275(11) Uani 1 1 d .
H8 H 0.4244 -0.3376 0.1097 0.033 Uiso 1 1 calc R
C9 C 0.4964(3) -0.2268(4) 0.1683(2) 0.0259(11) Uani 1 1 d .
C10 C 0.5843(4) -0.2939(5) 0.1615(3) 0.0364(13) Uani 1 1 d .
C11 C -0.0707(3) 0.8206(4) 0.0761(2) 0.0251(10) Uani 1 1 d .
C12 C -0.0213(3) 0.7331(4) 0.0358(2) 0.0198(10) Uani 1 1 d .
C13 C 0.0362(3) 0.7728(4) -0.0110(2) 0.0211(10) Uani 1 1 d .
H13 H 0.0402 0.8527 -0.0189 0.025 Uiso 1 1 calc R
C14 C 0.0876(3) 0.6977(4) -0.0463(2) 0.0209(10) Uani 1 1 d .
C15 C 0.1523(3) 0.7475(4) -0.0942(2) 0.0272(11) Uani 1 1 d .
C16 C 0.2245(3) 0.4141(4) 0.1896(2) 0.0195(9) Uani 1 1 d .
H16 H 0.2646 0.4042 0.2265 0.023 Uiso 1 1 calc R
C17 C 0.0858(3) 0.4638(4) 0.1462(2) 0.0190(9) Uani 1 1 d .
H17 H 0.0267 0.4906 0.1526 0.023 Uiso 1 1 calc R
C18 C 0.1910(3) 0.4050(4) 0.0765(2) 0.0204(10) Uani 1 1 d .
H18 H 0.2079 0.3873 0.0335 0.025 Uiso 1 1 calc R
C19 C 0.2544(3) 0.3907(4) 0.1282(2) 0.0182(9) Uani 1 1 d .
C20 C 0.3486(3) 0.3532(4) 0.1197(2) 0.0194(9) Uani 1 1 d .
C21 C 0.3912(3) 0.2846(4) 0.1667(2) 0.0198(9) Uani 1 1 d .
H21 H 0.3599 0.2614 0.2037 0.024 Uiso 1 1 calc R
C22 C 0.4800(3) 0.2491(4) 0.1600(2) 0.0179(9) Uani 1 1 d .
C23 C 0.5262(3) 0.2845(4) 0.1059(2) 0.0240(10) Uani 1 1 d .
H23 H 0.5866 0.2617 0.1011 0.029 Uiso 1 1 calc R
C24 C 0.4829(3) 0.3535(4) 0.0591(2) 0.0260(11) Uani 1 1 d .
H24 H 0.5143 0.3776 0.0222 0.031 Uiso 1 1 calc R
C25 C 0.3950(3) 0.3874(4) 0.0652(2) 0.0229(10) Uani 1 1 d .
H25 H 0.3661 0.4339 0.0325 0.027 Uiso 1 1 calc R
C26 C 0.6165(3) 0.1483(4) 0.2206(2) 0.0202(10) Uani 1 1 d .
C27 C 0.6260(3) 0.0807(5) 0.2849(2) 0.0255(11) Uani 1 1 d .
H27A H 0.5965 0.0062 0.2793 0.038 Uiso 1 1 calc R
H27B H 0.5977 0.1235 0.3195 0.038 Uiso 1 1 calc R
H27C H 0.6898 0.0693 0.2968 0.038 Uiso 1 1 calc R
C28 C 0.6637(3) 0.2640(4) 0.2294(2) 0.0263(11) Uani 1 1 d .
H28A H 0.6375 0.3061 0.2652 0.039 Uiso 1 1 calc R
H28B H 0.6561 0.3084 0.1890 0.039 Uiso 1 1 calc R
H28C H 0.7279 0.2516 0.2396 0.039 Uiso 1 1 calc R
C29 C 0.6527(3) 0.0755(4) 0.1660(2) 0.0263(11) Uani 1 1 d .
H29A H 0.6201 0.0028 0.1634 0.039 Uiso 1 1 calc R
H29B H 0.7167 0.0606 0.1752 0.039 Uiso 1 1 calc R
H29C H 0.6446 0.1164 0.1245 0.039 Uiso 1 1 calc R
F1 F 0.0851(2) 0.0292(3) 0.21191(16) 0.0455(9) Uani 1 1 d .
F2 F 0.0618(2) 0.0598(3) 0.11060(15) 0.0436(8) Uani 1 1 d .
F3 F 0.0852(2) 0.2006(3) 0.1756(2) 0.0606(11) Uani 1 1 d .
F4 F 0.2866(2) 0.0529(3) -0.03456(13) 0.0406(8) Uani 1 1 d .
F5 F 0.4212(2) 0.1045(3) -0.00794(15) 0.0479(9) Uani 1 1 d .
F6 F 0.3837(2) -0.0720(3) -0.00178(14) 0.0430(8) Uani 1 1 d .
F7 F 0.1916(2) -0.3107(3) 0.14236(16) 0.0473(9) Uani 1 1 d .
F8 F 0.2770(2) -0.3650(3) 0.06688(16) 0.0402(8) Uani 1 1 d .
F9 F 0.2194(2) -0.1974(3) 0.06339(16) 0.0426(8) Uani 1 1 d .
F10 F 0.6042(3) -0.3551(4) 0.21381(19) 0.0603(11) Uani 1 1 d .
F11 F 0.5824(3) -0.3641(4) 0.1106(2) 0.0718(14) Uani 1 1 d .
F12 F 0.6542(2) -0.2246(3) 0.1543(2) 0.0549(10) Uani 1 1 d .
F13 F -0.0294(2) 0.8328(3) 0.13499(13) 0.0353(7) Uani 1 1 d .
F14 F -0.15437(19) 0.7877(3) 0.08535(16) 0.0366(7) Uani 1 1 d .
F15 F -0.0752(2) 0.9239(2) 0.04790(14) 0.0311(7) Uani 1 1 d .
F16 F 0.1289(2) 0.7154(3) -0.15491(14) 0.0468(9) Uani 1 1 d .
F17 F 0.23528(19) 0.7085(3) -0.08125(16) 0.0395(8) Uani 1 1 d .
F18 F 0.1562(3) 0.8602(3) -0.0935(2) 0.0539(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
O2 Cu1 O7 93.36(13) . .
O2 Cu1 O3 88.02(13) . .
O7 Cu1 O3 175.90(13) . .
O2 Cu1 N1 169.67(14) . 2_545
O7 Cu1 N1 88.68(13) . 2_545
O3 Cu1 N1 89.28(14) . 2_545
O2 Cu1 O4 93.03(13) . .
O7 Cu1 O4 98.24(12) . .
O3 Cu1 O4 85.52(13) . .
N1 Cu1 O4 96.70(14) 2_545 .
O2 Cu1 O1 85.80(12) . .
O7 Cu1 O1 92.23(12) . .
O3 Cu1 O1 84.02(12) . .
N1 Cu1 O1 83.99(13) 2_545 .
O4 Cu1 O1 169.51(12) . .
O6 Cu2 O6 180.0(2) 3_565 .
O6 Cu2 O5 87.10(13) . 3_565
O6 Cu2 O5 92.90(13) . .
O5 Cu2 O5 180.0(2) 3_565 .
O6 Cu2 N3 87.00(13) 3_565 .
O6 Cu2 N3 93.00(13) . .
O5 Cu2 N3 88.05(13) 3_565 .
O5 Cu2 N3 91.95(13) . .
N3 Cu2 N3 180.0 . 3_565
C2 O1 Cu1 115.0(3) . .
C4 O2 Cu1 124.3(3) . .
C7 O3 Cu1 126.1(3) . .
C9 O4 Cu1 121.5(3) . .
C12 O5 Cu2 122.6(3) . .
C14 O6 Cu2 123.2(3) . .
N2 O7 Cu1 121.0(2) . .
C17 N1 C16 117.5(4) . .
C17 N1 Cu1 125.4(3) . 2
C16 N1 Cu1 117.0(3) . 2
O7 N2 C22 116.7(3) . .
O7 N2 C26 117.5(3) . .
C22 N2 C26 125.7(4) . .
C18 N3 C17 117.1(4) . .
C18 N3 Cu2 126.2(3) . .
C17 N3 Cu2 116.1(3) . .
F2 C1 F1 106.6(4) . .
F2 C1 F3 107.3(4) . .
F1 C1 F3 107.2(4) . .
F2 C1 C2 113.8(4) . .
F1 C1 C2 110.7(4) . .
F3 C1 C2 110.9(4) . .
O1 C2 C3 127.5(4) . .
O1 C2 C1 114.7(4) . .
C3 C2 C1 117.8(4) . .
C4 C3 C2 123.2(4) . .
O2 C4 C3 130.0(4) . .
O2 C4 C5 112.0(4) . .
C3 C4 C5 117.9(4) . .
F5 C5 F4 106.9(4) . .
F5 C5 F6 106.9(4) . .
F4 C5 F6 106.5(4) . .
F5 C5 C4 111.9(4) . .
F4 C5 C4 113.8(4) . .
F6 C5 C4 110.4(4) . .
F7 C6 F9 108.0(4) . .
F7 C6 F8 107.0(4) . .
F9 C6 F8 106.1(4) . .
F7 C6 C7 111.7(4) . .
F9 C6 C7 110.0(4) . .
F8 C6 C7 113.6(4) . .
O3 C7 C8 129.9(4) . .
O3 C7 C6 111.7(4) . .
C8 C7 C6 118.3(4) . .
C7 C8 C9 122.0(5) . .
O4 C9 C8 128.6(5) . .
O4 C9 C10 114.5(4) . .
C8 C9 C10 116.9(4) . .
F10 C10 F11 107.6(5) . .
F10 C10 F12 105.9(4) . .
F11 C10 F12 106.1(5) . .
F10 C10 C9 111.4(5) . .
F11 C10 C9 113.4(4) . .
F12 C10 C9 111.9(5) . .
F14 C11 F13 107.4(4) . .
F14 C11 F15 107.1(4) . .
F13 C11 F15 107.8(4) . .
F14 C11 C12 111.3(4) . .
F13 C11 C12 110.2(4) . .
F15 C11 C12 112.7(4) . .
O5 C12 C13 128.6(4) . .
O5 C12 C11 113.0(4) . .
C13 C12 C11 118.5(4) . .
C14 C13 C12 121.2(4) . .
O6 C14 C13 128.6(4) . .
O6 C14 C15 113.0(4) . .
C13 C14 C15 118.4(4) . .
F18 C15 F16 107.6(4) . .
F18 C15 F17 107.4(4) . .
F16 C15 F17 106.9(4) . .
F18 C15 C14 113.7(4) . .
F16 C15 C14 110.5(4) . .
F17 C15 C14 110.4(4) . .
N1 C16 C19 122.1(4) . .
N1 C17 N3 124.9(4) . .
N3 C18 C19 122.7(4) . .
C16 C19 C18 115.6(4) . .
C16 C19 C20 120.8(4) . .
C18 C19 C20 123.6(4) . .
C21 C20 C25 119.6(4) . .
C21 C20 C19 119.5(4) . .
C25 C20 C19 120.9(4) . .
C20 C21 C22 120.6(4) . .
C23 C22 C21 119.5(4) . .
C23 C22 N2 122.6(4) . .
C21 C22 N2 117.7(4) . .
C24 C23 C22 119.5(4) . .
C25 C24 C23 121.1(4) . .
C24 C25 C20 119.8(4) . .
N2 C26 C29 109.4(4) . .
N2 C26 C28 108.0(4) . .
C29 C26 C28 113.7(4) . .
N2 C26 C27 107.5(3) . .
C29 C26 C27 108.8(4) . .
C28 C26 C27 109.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.952(3) .
Cu1 O7 1.960(3) .
Cu1 O3 1.990(3) .
Cu1 N1 2.012(4) 2_545
Cu1 O4 2.254(3) .
Cu1 O1 2.325(3) .
Cu2 O6 1.949(3) .
Cu2 O5 1.957(3) .
Cu2 N3 2.415(4) .
O1 C2 1.235(5) .
O2 C4 1.269(5) .
O3 C7 1.259(6) .
O4 C9 1.247(6) .
O5 C12 1.262(6) .
O6 C14 1.256(6) .
O7 N2 1.300(5) .
N1 C17 1.329(6) .
N1 C16 1.347(6) .
N1 Cu1 2.012(4) 2
N2 C22 1.418(6) .
N2 C26 1.522(5) .
N3 C18 1.330(6) .
N3 C17 1.338(6) .
C1 F2 1.323(6) .
C1 F1 1.324(6) .
C1 F3 1.331(6) .
C1 C2 1.540(7) .
C2 C3 1.414(6) .
C3 C4 1.383(7) .
C4 C5 1.523(6) .
C5 F5 1.330(6) .
C5 F4 1.336(6) .
C5 F6 1.337(6) .
C6 F7 1.324(6) .
C6 F9 1.330(6) .
C6 F8 1.345(6) .
C6 C7 1.530(7) .
C7 C8 1.386(7) .
C8 C9 1.400(7) .
C9 C10 1.540(7) .
C10 F10 1.312(7) .
C10 F11 1.328(6) .
C10 F12 1.333(7) .
C11 F14 1.327(6) .
C11 F13 1.338(6) .
C11 F15 1.339(6) .
C11 C12 1.526(7) .
C12 C13 1.395(6) .
C13 C14 1.390(7) .
C14 C15 1.525(6) .
C15 F18 1.319(6) .
C15 F16 1.331(6) .
C15 F17 1.334(6) .
C16 C19 1.382(6) .
C18 C19 1.399(6) .
C19 C20 1.489(6) .
C20 C21 1.386(6) .
C20 C25 1.399(6) .
C21 C22 1.400(6) .
C22 C23 1.396(6) .
C23 C24 1.389(7) .
C24 C25 1.381(7) .
C26 C29 1.525(6) .
C26 C28 1.532(7) .
C26 C27 1.538(6) .
