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#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/16/7011650.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_7011650
loop_
_publ_author_name
'McMorran, David A.'
'Steel, Peter J.'
_publ_section_title
;
 New U- and Y-shaped components for metallosupramolecular assemblies:
 synthesis and coordination chemistry of 2,6-bis(3-pyridyloxy)pyrazine
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3321
_journal_paper_doi               10.1039/b202593k
_journal_year                    2002
_chemical_formula_sum            'C18 H17 B Cu F4 N6 O2.5'
_chemical_formula_weight         507.73
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           1
_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                95.96(3)
_cell_angle_beta                 107.60(2)
_cell_angle_gamma                116.67(2)
_cell_formula_units_Z            1
_cell_length_a                   8.211(7)
_cell_length_b                   8.327(7)
_cell_length_c                   9.356(6)
_cell_measurement_temperature    168(2)
_cell_volume                     522.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6286
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_T_max  0.9781
_exptl_absorpt_correction_T_min  0.6971
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             257
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         3059
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1139P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                2492
_reflns_number_total             3059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202593k.txt
_cod_data_source_block           3dmaaa
_cod_original_cell_volume        522.8(7)
_cod_original_formula_sum        'C18 H17 B Cu F4 N6 O2.50'
_cod_database_code               7011650
loop_
_symmetry_equiv_pos_as_xyz
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 1.44686(10) 0.42856(10) 0.32324(9) 0.0262(3) Uani 1 1 d . . .
N11 N 1.2540(9) 0.4514(9) 0.4037(7) 0.0261(15) Uani 1 1 d . . .
C12 C 1.2967(12) 0.4867(11) 0.5567(9) 0.0270(18) Uani 1 1 d . . .
H12A H 1.4219 0.5103 0.6256 0.032 Uiso 1 1 calc R . .
C13 C 1.1678(15) 0.4901(12) 0.6175(11) 0.027(2) Uani 1 1 d . . .
C14 C 0.9836(12) 0.4500(11) 0.5189(9) 0.0278(18) Uani 1 1 d . . .
H14A H 0.8892 0.4483 0.5584 0.033 Uiso 1 1 calc R . .
C15 C 0.9410(14) 0.4128(13) 0.3634(10) 0.033(2) Uani 1 1 d . . .
H15A H 0.8150 0.3843 0.2919 0.039 Uiso 1 1 calc R . .
C16 C 1.0785(12) 0.4164(11) 0.3100(10) 0.0282(18) Uani 1 1 d . . .
H16A H 1.0471 0.3928 0.2008 0.034 Uiso 1 1 calc R . .
O10 O 1.2222(10) 0.5428(9) 0.7744(7) 0.0301(15) Uani 1 1 d . . .
N21 N 1.1500(11) 0.2440(10) 0.7678(8) 0.0257(16) Uani 1 1 d . . .
C22 C 1.2232(14) 0.4143(13) 0.8501(11) 0.025(2) Uani 1 1 d . . .
C23 C 1.3109(13) 0.4721(12) 1.0093(10) 0.030(2) Uani 1 1 d . . .
H23A H 1.3626 0.5984 1.0637 0.036 Uiso 1 1 calc R . .
N24 N 1.3238(10) 0.3532(9) 1.0873(8) 0.0299(16) Uani 1 1 d . . .
C25 C 1.2566(12) 0.1814(11) 1.0072(9) 0.0301(19) Uani 1 1 d . . .
H25A H 1.2691 0.0933 1.0598 0.036 Uiso 1 1 calc R . .
C26 C 1.1686(11) 0.1306(11) 0.8479(9) 0.0275(18) Uani 1 1 d . . .
O20 O 1.0922(9) -0.0508(7) 0.7736(6) 0.0357(15) Uani 1 1 d . . .
N31 N 0.7133(9) -0.3401(9) 0.3997(7) 0.0242(15) Uani 1 1 d . . .
C32 C 0.8135(12) -0.2603(10) 0.5507(9) 0.0232(17) Uani 1 1 d . . .
H32A H 0.7515 -0.3094 0.6192 0.028 Uiso 1 1 calc R . .
C33 C 1.0012(13) -0.1111(11) 0.6139(9) 0.0303(19) Uani 1 1 d . . .
C34 C 1.0942(13) -0.0334(12) 0.5194(10) 0.034(2) Uani 1 1 d . . .
H34A H 1.2242 0.0728 0.5609 0.041 Uiso 1 1 calc R . .
C35 C 0.9913(13) -0.1157(12) 0.3630(10) 0.037(2) Uani 1 1 d . . .
H35A H 1.0495 -0.0685 0.2920 0.044 Uiso 1 1 calc R . .
C36 C 0.8031(12) -0.2671(11) 0.3083(10) 0.0310(19) Uani 1 1 d . . .
H36A H 0.7338 -0.3224 0.1986 0.037 Uiso 1 1 calc R . .
N40 N 1.4762(10) 0.2217(10) 0.3820(9) 0.0328(17) Uani 1 1 d . . .
C40 C 1.5059(15) 0.1116(14) 0.4192(12) 0.041(2) Uani 1 1 d . . .
C41 C 1.548(3) -0.0250(19) 0.4713(18) 0.082(4) Uani 1 1 d . . .
H41A H 1.6560 0.0332 0.5751 0.123 Uiso 1 1 calc R . .
H41B H 1.5872 -0.0769 0.3979 0.123 Uiso 1 1 calc R . .
H41C H 1.4293 -0.1257 0.4770 0.123 Uiso 1 1 calc R . .
N200 N 1.553(2) 0.9544(14) 1.1126(15) 0.078(3) Uani 1 1 d . . .
C201 C 1.6241(18) 0.9565(14) 1.0297(15) 0.057(3) Uani 1 1 d . . .
C202 C 1.715(3) 0.957(2) 0.923(2) 0.103(5) Uani 1 1 d . . .
H20A H 1.7501 1.0722 0.8903 0.154 Uiso 1 1 calc R . .
H20B H 1.6233 0.8482 0.8318 0.154 Uiso 1 1 calc R . .
H20C H 1.8355 0.9523 0.9740 0.154 Uiso 1 1 calc R . .
B B 0.6948(14) 0.3855(14) 0.8548(11) 0.042(3) Uani 1 1 d D . .
F1 F 0.5345(11) 0.2202(11) 0.7760(9) 0.101(3) Uani 1 1 d D A .
F2 F 0.729(3) 0.402(2) 1.0043(13) 0.115(9) Uani 0.71(4) 1 d PD A 1
F3 F 0.675(2) 0.5232(18) 0.818(2) 0.127(12) Uani 0.71(4) 1 d PD A 1
F4 F 0.8437(19) 0.387(2) 0.831(3) 0.163(12) Uani 0.71(4) 1 d PD A 1
F2' F 0.644(4) 0.489(4) 0.923(5) 0.22(5) Uani 0.29(4) 1 d PD A 2
F3' F 0.756(5) 0.461(4) 0.751(3) 0.13(2) Uani 0.29(4) 1 d PD A 2
F4' F 0.833(3) 0.374(3) 0.954(4) 0.17(4) Uani 0.29(4) 1 d PD A 2
O1 O 1.145(2) 0.7741(19) 1.1050(17) 0.054(4) Uani 0.50 1 d P . .
H1A H 1.0196 0.6362 1.0464 0.081 Uiso 0.50 1 d PR . .
H1B H 1.0749 0.7897 1.0915 0.081 Uiso 0.50 1 d PR . .
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'
B B 0.0013 0.0007 '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
_geom_angle_publ_flag
N40 Cu1 N31 109.6(3) . 1_665 ?
N40 Cu1 N11 107.8(3) . . ?
N31 Cu1 N11 114.9(3) 1_665 . ?
N40 Cu1 N24 106.5(3) . 1_554 ?
N31 Cu1 N24 109.4(3) 1_665 1_554 ?
N11 Cu1 N24 108.3(3) . 1_554 ?
C16 N11 C12 117.9(7) . . ?
C16 N11 Cu1 122.5(6) . . ?
C12 N11 Cu1 119.2(5) . . ?
N11 C12 C13 122.3(8) . . ?
C12 C13 O10 120.8(9) . . ?
C12 C13 C14 119.4(9) . . ?
O10 C13 C14 119.7(8) . . ?
C15 C14 C13 117.8(8) . . ?
C14 C15 C16 119.9(9) . . ?
N11 C16 C15 122.5(8) . . ?
C22 O10 C13 116.6(7) . . ?
C26 N21 C22 115.2(8) . . ?
N21 C22 O10 118.4(8) . . ?
N21 C22 C23 123.4(9) . . ?
O10 C22 C23 118.0(8) . . ?
N24 C23 C22 119.9(8) . . ?
C23 N24 C25 118.1(7) . . ?
C23 N24 Cu1 121.9(6) . 1_556 ?
C25 N24 Cu1 120.0(6) . 1_556 ?
N24 C25 C26 119.5(8) . . ?
N21 C26 O20 119.8(7) . . ?
N21 C26 C25 123.8(8) . . ?
O20 C26 C25 116.4(7) . . ?
C26 O20 C33 119.4(6) . . ?
C32 N31 C36 116.6(7) . . ?
C32 N31 Cu1 119.2(5) . 1_445 ?
C36 N31 Cu1 124.0(5) . 1_445 ?
N31 C32 C33 123.4(7) . . ?
C32 C33 C34 120.2(8) . . ?
C32 C33 O20 116.9(7) . . ?
C34 C33 O20 122.8(8) . . ?
C35 C34 C33 116.6(8) . . ?
C34 C35 C36 119.6(8) . . ?
N31 C36 C35 123.5(8) . . ?
C40 N40 Cu1 175.4(7) . . ?
N40 C40 C41 178.2(12) . . ?
N200 C201 C202 179.5(14) . . ?
F4' B F3 134.1(14) . . ?
F4' B F4 55.0(17) . . ?
F3 B F4 110.7(10) . . ?
F4' B F2' 111.0(13) . . ?
F3 B F2' 51.2(18) . . ?
F4 B F2' 143.3(15) . . ?
F4' B F3' 109.7(12) . . ?
F3 B F3' 58.0(15) . . ?
F4 B F3' 58.4(16) . . ?
F2' B F3' 108.4(13) . . ?
F4' B F2 54.1(19) . . ?
F3 B F2 109.4(10) . . ?
F4 B F2 108.3(11) . . ?
F2' B F2 62.2(19) . . ?
F3' B F2 146.6(14) . . ?
F4' B F1 112.9(11) . . ?
F3 B F1 113.0(9) . . ?
F4 B F1 108.4(10) . . ?
F2' B F1 108.2(11) . . ?
F3' B F1 106.5(11) . . ?
F2 B F1 106.9(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N40 1.954(8) . ?
Cu1 N31 1.998(7) 1_665 ?
Cu1 N11 2.018(7) . ?
Cu1 N24 2.020(7) 1_554 ?
N11 C16 1.318(11) . ?
N11 C12 1.332(10) . ?
C12 C13 1.353(13) . ?
C13 O10 1.356(11) . ?
C13 C14 1.374(13) . ?
C14 C15 1.354(11) . ?
C15 C16 1.356(12) . ?
O10 C22 1.345(11) . ?
N21 C26 1.298(11) . ?
N21 C22 1.301(11) . ?
C22 C23 1.364(13) . ?
C23 N24 1.312(11) . ?
N24 C25 1.315(10) . ?
N24 Cu1 2.020(7) 1_556 ?
C25 C26 1.366(11) . ?
C26 O20 1.351(10) . ?
O20 C33 1.369(10) . ?
N31 C32 1.313(10) . ?
N31 C36 1.315(10) . ?
N31 Cu1 1.998(7) 1_445 ?
C32 C33 1.358(11) . ?
C33 C34 1.366(12) . ?
C34 C35 1.360(12) . ?
C35 C36 1.370(12) . ?
N40 C40 1.113(11) . ?
C40 C41 1.419(15) . ?
N200 C201 1.102(15) . ?
C201 C202 1.414(19) . ?
B F4' 1.281(14) . ?
B F3 1.295(12) . ?
B F4 1.303(11) . ?
B F2' 1.309(14) . ?
B F3' 1.315(14) . ?
B F2 1.320(12) . ?
B F1 1.322(10) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N40 Cu1 N11 C16 -113.5(6) . . . . ?
N31 Cu1 N11 C16 123.9(6) 1_665 . . . ?
N24 Cu1 N11 C16 1.4(7) 1_554 . . . ?
N40 Cu1 N11 C12 60.3(6) . . . . ?
N31 Cu1 N11 C12 -62.3(6) 1_665 . . . ?
N24 Cu1 N11 C12 175.1(6) 1_554 . . . ?
C16 N11 C12 C13 -0.9(12) . . . . ?
Cu1 N11 C12 C13 -175.0(7) . . . . ?
N11 C12 C13 O10 -174.1(8) . . . . ?
N11 C12 C13 C14 2.2(13) . . . . ?
C12 C13 C14 C15 -1.6(12) . . . . ?
O10 C13 C14 C15 174.7(8) . . . . ?
C13 C14 C15 C16 -0.1(13) . . . . ?
C12 N11 C16 C15 -0.9(12) . . . . ?
Cu1 N11 C16 C15 173.0(6) . . . . ?
C14 C15 C16 N11 1.4(13) . . . . ?
C12 C13 O10 C22 -78.6(11) . . . . ?
C14 C13 O10 C22 105.1(10) . . . . ?
C26 N21 C22 O10 175.2(8) . . . . ?
C26 N21 C22 C23 -1.1(14) . . . . ?
C13 O10 C22 N21 -8.2(13) . . . . ?
C13 O10 C22 C23 168.2(8) . . . . ?
N21 C22 C23 N24 -0.3(15) . . . . ?
O10 C22 C23 N24 -176.6(8) . . . . ?
C22 C23 N24 C25 2.3(13) . . . . ?
C22 C23 N24 Cu1 -178.7(7) . . . 1_556 ?
C23 N24 C25 C26 -2.9(12) . . . . ?
Cu1 N24 C25 C26 178.1(6) 1_556 . . . ?
C22 N21 C26 O20 178.1(8) . . . . ?
C22 N21 C26 C25 0.5(13) . . . . ?
N24 C25 C26 N21 1.5(13) . . . . ?
N24 C25 C26 O20 -176.1(7) . . . . ?
N21 C26 O20 C33 1.9(12) . . . . ?
C25 C26 O20 C33 179.7(8) . . . . ?
C36 N31 C32 C33 -0.7(11) . . . . ?
Cu1 N31 C32 C33 175.0(6) 1_445 . . . ?
N31 C32 C33 C34 1.5(13) . . . . ?
N31 C32 C33 O20 -175.6(7) . . . . ?
C26 O20 C33 C32 -125.7(8) . . . . ?
C26 O20 C33 C34 57.3(12) . . . . ?
C32 C33 C34 C35 -1.6(13) . . . . ?
O20 C33 C34 C35 175.4(8) . . . . ?
C33 C34 C35 C36 0.9(13) . . . . ?
C32 N31 C36 C35 0.0(12) . . . . ?
Cu1 N31 C36 C35 -175.5(7) 1_445 . . . ?
C34 C35 C36 N31 -0.1(13) . . . . ?
N31 Cu1 N40 C40 -5(9) 1_665 . . . ?
N11 Cu1 N40 C40 -130(9) . . . . ?
N24 Cu1 N40 C40 114(9) 1_554 . . . ?
Cu1 N40 C40 C41 52(43) . . . . ?
