#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/55/7005597.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_7005597
loop_
_publ_author_name
'Hoffart, Dennis J.'
'Habermehl, Nicolle C.'
'Loeb, Stephen J.'
_publ_section_title
;
 4,4'-Bipyridine-N-monoxide. A hybrid ligand for building networks
 using a combination of metal-ligand and hydrogen-bonding interactions.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2870
_journal_page_last               2875
_journal_paper_doi               10.1039/b703456c
_journal_year                    2007
_chemical_formula_sum            'C40 H39 Cu F12 N8 O7.5 P2'
_chemical_formula_weight         1105.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           104
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.183(8)
_cell_length_b                   17.183(8)
_cell_length_c                   8.128(6)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      1.5
_cell_volume                     2400(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'hemisphere 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  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18137
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_number         100
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.857200
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blue
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2113
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.084
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0707P)²+5.9652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1719
_reflns_number_gt                1777
_reflns_number_total             2113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b703456c.txt
_cod_data_source_block           '[Cu(H2O)2(BIPYMO)4][PF6]2'
_cod_original_sg_symbol_H-M      P4nc
_cod_original_formula_sum        'C40 H39 Cu F12 N8 O7.50 P2'
_cod_database_code               7005597
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.0000 -0.0035(3) 0.0273(4) Uani 1 4 d S . .
O1 O 0.4884(2) -0.3560(3) -0.0400(13) 0.104(4) Uani 1 1 d . . .
O1W O 0.0000 0.0000 -0.2970(14) 0.041(3) Uani 1 4 d S . .
H1W H -0.0012 -0.0461 -0.3314 0.049 Uiso 0.50 1 calc PR . .
O2W O 0.0000 0.0000 0.2770(13) 0.040(3) Uani 1 4 d S . .
H2W H -0.0004 -0.0461 0.3114 0.047 Uiso 0.50 1 calc PR . .
N1 N 0.1003(2) -0.0641(2) -0.0034(9) 0.0298(10) Uani 1 1 d . . .
N2 N 0.4284(3) -0.3090(3) -0.0290(12) 0.065(2) Uani 1 1 d . . .
C1 C 0.1605(3) -0.0483(3) -0.1019(9) 0.0353(14) Uani 1 1 d . . .
H1A H 0.1569 -0.0047 -0.1734 0.042 Uiso 1 1 calc R . .
C2 C 0.2280(4) -0.0925(3) -0.1048(9) 0.0384(15) Uani 1 1 d . . .
H2A H 0.2699 -0.0788 -0.1754 0.046 Uiso 1 1 calc R . .
C3 C 0.2334(3) -0.1575(3) -0.0019(12) 0.0334(12) Uani 1 1 d . . .
C4 C 0.1721(4) -0.1730(4) 0.1002(8) 0.0365(14) Uani 1 1 d . . .
H4A H 0.1740 -0.2163 0.1727 0.044 Uiso 1 1 calc R . .
C5 C 0.1073(4) -0.1255(3) 0.0976(8) 0.0352(15) Uani 1 1 d . . .
H5A H 0.0657 -0.1368 0.1707 0.042 Uiso 1 1 calc R . .
C6 C 0.3024(3) -0.2094(3) -0.0107(13) 0.0377(13) Uani 1 1 d . . .
C7 C 0.3751(4) -0.1831(4) -0.0557(10) 0.051(2) Uani 1 1 d . . .
H7A H 0.3824 -0.1297 -0.0820 0.062 Uiso 1 1 calc R . .
C8 C 0.4381(4) -0.2342(4) -0.0631(13) 0.068(3) Uani 1 1 d . . .
H8A H 0.4882 -0.2153 -0.0926 0.082 Uiso 1 1 calc R . .
C9 C 0.3583(3) -0.3365(3) 0.0211(12) 0.047(2) Uani 1 1 d . . .
H9A H 0.3529 -0.3894 0.0526 0.056 Uiso 1 1 calc R . .
C10 C 0.2958(4) -0.2878(4) 0.0262(10) 0.044(2) Uani 1 1 d . . .
H10A H 0.2463 -0.3082 0.0557 0.053 Uiso 1 1 calc R . .
P1 P 0.0827(3) -0.3845(4) -0.2326(9) 0.100(2) Uani 0.50 1 d PDU A -1
F1 F 0.1098(13) -0.3932(14) -0.4150(17) 0.243(10) Uani 0.50 1 d PDU A -1
F2 F 0.1669(8) -0.3778(13) -0.175(3) 0.208(11) Uani 0.50 1 d PDU A -1
F3 F 0.0895(12) -0.4758(7) -0.217(4) 0.286(13) Uani 0.50 1 d PDU A -1
F4 F 0.0746(8) -0.2976(6) -0.254(2) 0.177(8) Uani 0.50 1 d PDU A -1
F5 F -0.0027(6) -0.3984(10) -0.289(3) 0.219(10) Uani 0.50 1 d PDU A -1
F6 F 0.0514(15) -0.3797(15) -0.0550(19) 0.325(13) Uani 0.50 1 d PDU A -1
O1S O 0.157(2) -0.390(3) -0.269(7) 0.27(3) Uani 0.50 1 d PD B -2
O2S O 0.028(2) -0.436(2) -0.465(8) 0.18(2) Uani 0.25 1 d PD C -2
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'
P P 0.1023 0.0942 '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
N1 Cu1 N1 179.9(4) 4 3 ?
N1 Cu1 N1 90.0 4 . ?
N1 Cu1 N1 90.0 3 . ?
N1 Cu1 N1 90.0 4 2 ?
N1 Cu1 N1 90.0 3 2 ?
N1 Cu1 N1 179.9(4) . 2 ?
N1 Cu1 O2W 90.0(2) 4 . ?
N1 Cu1 O2W 90.0(2) 3 . ?
N1 Cu1 O2W 90.0(2) . . ?
N1 Cu1 O2W 90.0(2) 2 . ?
N1 Cu1 O1W 90.0(2) 4 . ?
N1 Cu1 O1W 90.0(2) 3 . ?
N1 Cu1 O1W 90.0(2) . . ?
N1 Cu1 O1W 90.0(2) 2 . ?
O2W Cu1 O1W 180 . . ?
C1 N1 C5 117.2(5) . . ?
C1 N1 Cu1 122.9(4) . . ?
C5 N1 Cu1 119.9(4) . . ?
O1 N2 C8 118.9(6) . . ?
O1 N2 C9 120.3(6) . . ?
C8 N2 C9 120.8(6) . . ?
N1 C1 C2 123.1(6) . . ?
C1 C2 C3 118.8(6) . . ?
C4 C3 C2 117.9(5) . . ?
C4 C3 C6 121.8(6) . . ?
C2 C3 C6 120.2(7) . . ?
C3 C4 C5 119.8(6) . . ?
N1 C5 C4 123.1(6) . . ?
C7 C6 C10 116.8(5) . . ?
C7 C6 C3 122.6(5) . . ?
C10 C6 C3 120.6(6) . . ?
C6 C7 C8 120.5(7) . . ?
N2 C8 C7 120.2(7) . . ?
N2 C9 C10 119.7(6) . . ?
C9 C10 C6 121.7(6) . . ?
F2 P1 F4 92.8(8) . . ?
F2 P1 F6 92.2(8) . . ?
F4 P1 F6 91.4(8) . . ?
F2 P1 F5 175.5(9) . . ?
F4 P1 F5 91.7(7) . . ?
F6 P1 F5 87.4(7) . . ?
F2 P1 F1 91.0(7) . . ?
F4 P1 F1 90.7(8) . . ?
F6 P1 F1 176.1(10) . . ?
F5 P1 F1 89.2(8) . . ?
F2 P1 F3 88.9(7) . . ?
F4 P1 F3 177.6(9) . . ?
F6 P1 F3 90.2(8) . . ?
F5 P1 F3 86.6(7) . . ?
F1 P1 F3 87.6(8) . . ?
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 N1 2.046(4) 4 ?
Cu1 N1 2.046(4) 3 ?
Cu1 N1 2.046(4) . ?
Cu1 N1 2.046(4) 2 ?
Cu1 O2W 2.280(11) . ?
Cu1 O1W 2.385(12) . ?
O1 N2 1.312(7) . ?
N1 C1 1.335(8) . ?
N1 C5 1.342(8) . ?
N2 C8 1.326(10) . ?
N2 C9 1.355(9) . ?
C1 C2 1.387(8) . ?
C2 C3 1.399(9) . ?
C3 C4 1.367(10) . ?
C3 C6 1.485(7) . ?
C4 C5 1.380(9) . ?
C6 C7 1.378(9) . ?
C6 C10 1.385(9) . ?
C7 C8 1.396(9) . ?
C9 C10 1.362(9) . ?
P1 F2 1.525(11) . ?
P1 F4 1.509(10) . ?
P1 F6 1.543(11) . ?
P1 F5 1.556(10) . ?
P1 F1 1.560(10) . ?
P1 F3 1.579(11) . ?
