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#$Date: 2016-03-23 15:19:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179322 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/19/4321971.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_4321971
loop_
_publ_author_name
'Hongyan Luo'
'Jem-Mau Lo'
'Phillip E. Fanwick'
'Joseph G. Stowell'
'Mark A. Green'
_publ_contact_author_address
;    Department of Medicinal Chemistry and Molecular Pharmacology
     Purdue University
     W. Lafayette
     IN 47907
     USA
;
_publ_contact_author_email       magreen@pharmacy.purdue.edu
_publ_contact_author_fax         1(765)4941414
_publ_contact_author_name        'Mark A. Green'
_publ_contact_author_phone       1(765)4941441
_publ_section_title
;
 Monoprotic Tetradentate N3O-Donor Ligands and Their Cu(II) and Ni(II)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2071
_journal_page_last               2078
_journal_paper_doi               10.1021/ic981324f
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C34 H44 B2 Cu2 F8 N6 O2'
_chemical_formula_weight         869.46
_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_type_scat_source
'International Tables for Crystallography (Vol C) '
_cell_angle_alpha                107.200(3)
_cell_angle_beta                 91.193(2)
_cell_angle_gamma                105.052(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1471(4)
_cell_length_b                   10.3753(3)
_cell_length_c                   10.5352(5)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    296
_cell_measurement_theta_max      30
_cell_measurement_theta_min      4
_cell_volume                     917.17(7)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    Xtal_GX (Hall, 1995)
    PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    PATTY_(DIRDIF92,_Beurskins,_1992)
_diffrn_ambient_temperature      296
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9644
_diffrn_reflns_theta_max         30.39
_diffrn_reflns_theta_min         4.47
_exptl_absorpt_coefficient_mu    1.241
_exptl_absorpt_correction_T_max  0.9055
_exptl_absorpt_correction_T_min  0.6507
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_description       plate
_exptl_crystal_F_000             446
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.93
_refine_ls_extinction_coef       0.58E-01
_refine_ls_extinction_method     SHELXL97_(Sheldrick_1997)
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4613
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.074
_refine_ls_shift/su_max          0.078
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1479P)²+0.5925P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.208
_reflns_number_gt                3306
_reflns_number_total             4613
_reflns_threshold_expression     >2.0σ(I)
_cod_data_source_file            ic981324f_2.cif
_cod_data_source_block           '[Cu(pamap)]2(BF4)2_(RL_373)'
_cod_original_cell_volume        917.17(14)
_cod_database_code               4321971
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
Cu 0.14347(6) 0.09826(5) 0.11604(5) 0.0401(2) Uani ?
F(1) 0.582(3) 0.1482(12) 0.358(2) 0.424(14) Uani ?
F(2) 0.6993(10) 0.3003(13) 0.5334(9) 0.214(6) Uani ?
F(3) 0.4977(10) 0.2960(14) 0.4319(14) 0.230(8) Uani ?
F(4) 0.7070(9) 0.3412(14) 0.3536(9) 0.213(6) Uani ?
O(20) 0.1042(4) 0.0592(3) -0.0736(3) 0.0396(9) Uani ?
N(1) 0.2570(4) -0.0495(4) 0.0915(4) 0.0421(12) Uani ?
N(8) 0.1820(5) 0.1127(5) 0.3101(4) 0.0465(12) Uani ?
N(12) 0.1388(5) 0.3050(4) 0.1649(4) 0.0457(12) Uani ?
C(2) 0.3185(6) -0.1052(5) -0.0177(5) 0.0452(12) Uani ?
C(3) 0.3897(6) -0.2089(5) -0.0272(6) 0.0535(18) Uani ?
C(4) 0.3970(7) -0.2569(5) 0.0839(6) 0.0589(18) Uani ?
C(5) 0.3332(7) -0.1986(6) 0.1967(6) 0.0585(18) Uani ?
C(6) 0.2628(5) -0.0965(5) 0.1967(5) 0.0450(12) Uani ?
C(7) 0.1858(6) -0.0277(6) 0.3141(5) 0.0515(16) Uani ?
C(9) 0.0756(7) 0.1710(6) 0.3978(5) 0.0595(16) Uani ?
C(10) 0.0912(7) 0.3227(6) 0.4063(6) 0.064(2) Uani ?
C(11) 0.0442(7) 0.3423(6) 0.2770(6) 0.0620(18) Uani ?
C(12) 0.2991(6) 0.3971(5) 0.2016(6) 0.0543(18) Uani ?
C(13) 0.0729(6) 0.3311(5) 0.0476(5) 0.0518(16) Uani ?
C(14) 0.1531(6) 0.2962(5) -0.0751(5) 0.0486(16) Uani ?
C(15) 0.2155(7) 0.3970(6) -0.1382(7) 0.065(2) Uani ?
C(16) 0.2912(8) 0.3670(8) -0.2489(7) 0.079(2) Uani ?
C(17) 0.3111(7) 0.2343(8) -0.2982(6) 0.068(2) Uani ?
C(18) 0.2500(6) 0.1294(6) -0.2391(5) 0.0526(16) Uani ?
C(19) 0.1677(5) 0.1607(5) -0.1289(5) 0.0435(12) Uani ?
B 0.6225(7) 0.2606(8) 0.4209(6) 0.062(2) Uani ?
H(2) 0.3131 -0.0726 -0.0905 0.0590 Uiso calc
H(3) 0.4317 -0.2460 -0.1046 0.0700 Uiso calc
H(4) 0.4441 -0.3269 0.0814 0.0760 Uiso calc
H(5) 0.3378 -0.2280 0.2716 0.0760 Uiso calc
H(8) 0.274(7) 0.179(6) 0.346(6) 0.0600 Uiso ?
H(15) 0.2049 0.4872 -0.1033 0.0850 Uiso calc
H(16) 0.3287 0.4347 -0.2904 0.1030 Uiso calc
H(17) 0.3656 0.2139 -0.3716 0.0880 Uiso calc
H(18) 0.2642 0.0405 -0.2728 0.0680 Uiso calc
H(7A) 0.0829 -0.0859 0.3101 0.0670 Uiso calc
H(7B) 0.2413 -0.0186 0.3972 0.0670 Uiso calc
H(9A) 0.0956 0.1657 0.4866 0.0770 Uiso calc
H(9B) -0.0280 0.1150 0.3635 0.0770 Uiso calc
H(10A) 0.0298 0.3604 0.4738 0.0830 Uiso calc
H(10B) 0.1965 0.3767 0.4353 0.0830 Uiso calc
H(11A) -0.0602 0.2859 0.2474 0.0800 Uiso calc
H(11B) 0.0457 0.4399 0.2947 0.0800 Uiso calc
H(12A) 0.2988 0.4938 0.2273 0.0710 Uiso calc
H(12B) 0.3561 0.3775 0.1261 0.0710 Uiso calc
H(12C) 0.3451 0.3790 0.2748 0.0710 Uiso calc
H(13A) 0.0751 0.4295 0.0720 0.0680 Uiso calc
H(13B) -0.0329 0.2761 0.0266 0.0680 Uiso calc
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(20) Cu N(8) 172.64(14) ?
O(20) Cu N(1) 92.42(15) ?
N(8) Cu N(1) 81.52(17) ?
O(20) Cu N(12) 95.14(15) ?
N(8) Cu N(12) 92.17(17) ?
N(1) Cu N(12) 151.55(16) ?
O(20) Cu O(20) 79.08(13) ?
N(8) Cu O(20) 97.35(14) ?
N(1) Cu O(20) 96.27(13) ?
N(12) Cu O(20) 112.08(14) ?
C(19) O(20) Cu 118.8(3) ?
C(19) O(20) Cu 130.2(3) ?
Cu O(20) Cu 100.92(13) ?
C(2) N(1) C(6) 119.2(4) ?
C(2) N(1) Cu 126.6(3) ?
C(6) N(1) Cu 114.1(3) ?
C(9) N(8) C(7) 113.2(4) ?
C(9) N(8) Cu 114.7(3) ?
C(7) N(8) Cu 107.3(3) ?
C(13) N(12) C(12) 108.1(4) ?
C(13) N(12) C(11) 107.6(4) ?
C(12) N(12) C(11) 110.4(4) ?
C(13) N(12) Cu 110.1(3) ?
C(12) N(12) Cu 108.4(3) ?
C(11) N(12) Cu 112.1(3) ?
N(1) C(2) C(3) 122.7(5) ?
C(2) C(3) C(4) 117.9(5) ?
C(5) C(4) C(3) 119.0(5) ?
C(6) C(5) C(4) 119.1(5) ?
N(1) C(6) C(5) 122.0(5) ?
N(1) C(6) C(7) 114.5(4) ?
C(5) C(6) C(7) 123.4(5) ?
N(8) C(7) C(6) 109.8(4) ?
N(8) C(9) C(10) 111.6(5) ?
C(11) C(10) C(9) 114.2(5) ?
N(12) C(11) C(10) 116.3(5) ?
N(12) C(13) C(14) 114.4(4) ?
C(19) C(14) C(15) 118.6(5) ?
C(19) C(14) C(13) 119.7(4) ?
C(15) C(14) C(13) 121.7(5) ?
C(16) C(15) C(14) 122.3(6) ?
C(15) C(16) C(17) 118.9(5) ?
C(16) C(17) C(18) 121.0(6) ?
C(19) C(18) C(17) 119.2(6) ?
O(20) C(19) C(14) 120.3(4) ?
O(20) C(19) C(18) 119.8(4) ?
C(14) C(19) C(18) 120.0(5) ?
F(1) B F(2) 122.9(17) ?
F(1) B F(3) 101.9(15) ?
F(2) B F(3) 110.8(10) ?
F(1) B F(4) 111.5(14) ?
F(2) B F(4) 103.6(8) ?
F(3) B F(4) 105.1(9) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cu O(20) 1.924(3) ?
Cu N(8) 2.022(4) ?
Cu N(1) 2.025(4) ?
Cu N(12) 2.064(4) ?
Cu O(20) 2.367(3) ?
F(1) B 1.116(11) ?
F(2) B 1.263(10) ?
F(3) B 1.284(10) ?
F(4) B 1.355(11) ?
O(20) C(19) 1.358(5) ?
O(20) Cu 2.367(3) ?
N(1) C(2) 1.333(6) ?
N(1) C(6) 1.342(6) ?
N(8) C(9) 1.477(7) ?
N(8) C(7) 1.479(7) ?
N(12) C(13) 1.489(7) ?
N(12) C(12) 1.498(6) ?
N(12) C(11) 1.497(7) ?
C(2) C(3) 1.377(7) ?
C(3) C(4) 1.409(8) ?
C(4) C(5) 1.380(9) ?
C(5) C(6) 1.375(7) ?
C(6) C(7) 1.520(7) ?
C(9) C(10) 1.518(9) ?
C(10) C(11) 1.505(9) ?
C(13) C(14) 1.497(8) ?
C(14) C(19) 1.395(7) ?
C(14) C(15) 1.406(7) ?
C(15) C(16) 1.367(10) ?
C(16) C(17) 1.382(11) ?
C(17) C(18) 1.408(8) ?
C(18) C(19) 1.400(7) ?
