#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:19:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179322 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/19/4321904.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_4321904
loop_
_publ_author_name
'Susan Lopez'
'Steven W. Keller'
_publ_contact_author
;
 Steven W. Keller
 123 Chemistry
 Department of Chemistry
 University of Missouri- Columbia
 Columbia, MO 65211
;
_publ_contact_author_email       chemsk@showme.missouri.edu
_publ_section_title
;
 New Linear Coordination Polymers Based on Copper(I) and
 4,7-Phenanthroline: Structure Dependence on Solvent and Counteranion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1883
_journal_page_last               1888
_journal_paper_doi               10.1021/ic980800z
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         '[Cu1 (C12 H8 N2)(C7 H5 N1)2] P1 F6'
_chemical_formula_sum            'C38 H26 Cu2 F12 N6 P2'
_chemical_formula_weight         983.67
_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
_cell_angle_alpha                115.700(2)
_cell_angle_beta                 98.810(2)
_cell_angle_gamma                96.020(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7480(10)
_cell_length_b                   12.5750(11)
_cell_length_c                   14.1390(13)
_cell_measurement_temperature    173(2)
_cell_volume                     1825.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3712
_diffrn_reflns_theta_full        20.86
_diffrn_reflns_theta_max         20.86
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    1.355
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube-like
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         3712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0984P)²+11.6459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1984
_reflns_number_gt                2668
_reflns_number_total             3712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980800z_3.cif
_cod_data_source_block           structure5
_cod_database_code               4321904
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.84358(13) 1.25581(13) 0.45498(12) 0.0396(5) Uani 1 1 d . . .
Cu2 Cu 0.79205(12) 0.58991(12) 0.12194(11) 0.0341(5) Uani 1 1 d . . .
P1 P 0.5160(3) 0.9061(3) 0.3203(3) 0.0487(10) Uani 1 1 d . . .
P2 P 0.1219(3) 0.3951(3) 0.3114(3) 0.0550(11) Uani 1 1 d . . .
F1 F 0.5813(9) 0.9377(13) 0.2458(9) 0.141(5) Uani 1 1 d . . .
F2 F 0.6110(7) 1.0045(7) 0.4203(6) 0.077(3) Uani 1 1 d . . .
F3 F 0.4280(6) 0.9951(6) 0.3336(6) 0.059(2) Uani 1 1 d . . .
F4 F 0.6065(10) 0.8169(10) 0.3120(10) 0.137(4) Uani 1 1 d . . .
F5 F 0.4270(8) 0.8050(7) 0.2149(6) 0.087(3) Uani 1 1 d . . .
F6 F 0.4649(11) 0.8481(9) 0.3828(7) 0.119(4) Uani 1 1 d . . .
F7 F 0.1962(9) 0.4777(11) 0.2854(13) 0.172(7) Uani 1 1 d . . .
F8 F 0.2182(7) 0.4015(8) 0.4012(7) 0.085(3) Uani 1 1 d . . .
F9 F 0.0676(7) 0.4954(7) 0.3908(7) 0.086(3) Uani 1 1 d . . .
F10 F 0.1791(9) 0.2954(9) 0.2271(8) 0.110(3) Uani 1 1 d . . .
F11 F 0.0244(9) 0.3853(10) 0.2173(7) 0.112(4) Uani 1 1 d . . .
F12 F 0.0363(8) 0.2916(8) 0.3066(9) 0.103(3) Uani 1 1 d . . .
N1 N 0.6543(8) 0.5455(8) 0.1849(7) 0.033(2) Uani 1 1 d . . .
N2 N 0.9808(8) 1.1924(8) 0.4603(7) 0.032(2) Uani 1 1 d . . .
N3 N 0.7020(8) 1.3041(8) 0.4320(7) 0.033(2) Uani 1 1 d . . .
N4 N 0.9477(8) 0.6999(8) 0.2280(7) 0.027(2) Uani 1 1 d . . .
N5 N 0.7161(9) 0.6694(9) 0.0397(8) 0.041(3) Uani 1 1 d . . .
N6 N 0.8341(9) 0.4332(10) 0.0294(8) 0.041(3) Uani 1 1 d . . .
C1 C 0.8935(11) 0.2220(11) -0.0533(9) 0.033(3) Uani 1 1 d . . .
C2 C 0.8094(10) 0.1229(11) -0.1253(9) 0.033(3) Uani 1 1 d . . .
H2 H 0.7310 0.1311 -0.1446 0.040 Uiso 1 1 calc R . .
C3 C 0.8406(12) 0.0117(11) -0.1687(9) 0.043(3) Uani 1 1 d . . .
H3 H 0.7840 -0.0573 -0.2195 0.052 Uiso 1 1 calc R . .
C4 C 0.9548(12) 0.0011(11) -0.1381(10) 0.041(3) Uani 1 1 d . . .
H4 H 0.9757 -0.0760 -0.1673 0.049 Uiso 1 1 calc R . .
C5 C 1.0381(11) 0.0994(11) -0.0667(10) 0.043(3) Uani 1 1 d . . .
H5 H 1.1165 0.0909 -0.0476 0.052 Uiso 1 1 calc R . .
C6 C 1.0078(11) 0.2113(11) -0.0223(9) 0.038(3) Uani 1 1 d . . .
H6 H 1.0645 0.2800 0.0287 0.045 Uiso 1 1 calc R . .
C7 C 0.8613(10) 0.3408(12) -0.0057(9) 0.033(3) Uani 1 1 d . . .
C8 C 0.6600(11) 0.7188(10) 0.0036(9) 0.035(3) Uani 1 1 d . . .
C9 C 0.5849(10) 0.7779(9) -0.0395(9) 0.029(3) Uani 1 1 d . . .
C10 C 0.4693(11) 0.7784(10) -0.0248(9) 0.039(3) Uani 1 1 d . . .
H10 H 0.4415 0.7427 0.0164 0.046 Uiso 1 1 calc R . .
C11 C 0.3977(11) 0.8298(11) -0.0696(9) 0.041(3) Uani 1 1 d . . .
H11 H 0.3200 0.8310 -0.0584 0.049 Uiso 1 1 calc R . .
C12 C 0.4349(11) 0.8796(11) -0.1301(9) 0.040(3) Uani 1 1 d . . .
H12 H 0.3827 0.9138 -0.1619 0.048 Uiso 1 1 calc R . .
C13 C 0.5471(12) 0.8810(10) -0.1457(9) 0.039(3) Uani 1 1 d . . .
H13 H 0.5732 0.9170 -0.1873 0.047 Uiso 1 1 calc R . .
C14 C 0.6223(10) 0.8293(10) -0.1003(9) 0.035(3) Uani 1 1 d . . .
H14 H 0.7000 0.8294 -0.1112 0.042 Uiso 1 1 calc R . .
C15 C 0.5523(11) 0.5769(10) 0.1632(9) 0.040(3) Uani 1 1 d . . .
H15 H 0.5476 0.6192 0.1215 0.048 Uiso 1 1 calc R . .
C16 C 0.4524(11) 0.5523(10) 0.1973(10) 0.041(3) Uani 1 1 d . . .
H16 H 0.3806 0.5726 0.1758 0.050 Uiso 1 1 calc R . .
C17 C 0.4609(10) 0.4985(10) 0.2620(9) 0.038(3) Uani 1 1 d . . .
H17 H 0.3949 0.4832 0.2887 0.045 Uiso 1 1 calc R . .
C18 C 0.5663(10) 0.4648(9) 0.2902(9) 0.029(3) Uani 1 1 d . . .
C19 C 0.6621(9) 0.4884(9) 0.2486(8) 0.025(3) Uani 1 1 d . . .
C20 C 0.7692(9) 0.4555(9) 0.2722(8) 0.024(3) Uani 1 1 d . . .
H20 H 0.8336 0.4744 0.2453 0.029 Uiso 1 1 calc R . .
C21 C 0.7816(9) 0.3966(9) 0.3333(8) 0.028(3) Uani 1 1 d . . .
H21 H 0.8547 0.3753 0.3492 0.033 Uiso 1 1 calc R . .
C22 C 1.0431(11) 0.6538(10) 0.2314(9) 0.035(3) Uani 1 1 d . . .
H22 H 1.0347 0.5691 0.1911 0.041 Uiso 1 1 calc R . .
C23 C 1.1549(9) 0.7188(11) 0.2891(9) 0.030(3) Uani 1 1 d . . .
H23 H 1.2200 0.6800 0.2887 0.036 Uiso 1 1 calc R . .
C24 C 1.1675(9) 0.8385(11) 0.3454(8) 0.030(3) Uani 1 1 d . . .
H24 H 1.2434 0.8854 0.3843 0.036 Uiso 1 1 calc R . .
C25 C 1.0715(10) 0.8952(10) 0.3478(8) 0.026(3) Uani 1 1 d . . .
C26 C 0.9617(9) 0.8210(10) 0.2875(8) 0.021(3) Uani 1 1 d . . .
C27 C 0.8615(9) 0.8763(10) 0.2888(8) 0.026(3) Uani 1 1 d . . .
H27 H 0.7870 0.8269 0.2484 0.031 Uiso 1 1 calc R . .
C28 C 0.8686(10) 0.9964(10) 0.3454(8) 0.028(3) Uani 1 1 d . . .
H28 H 0.7998 1.0301 0.3454 0.034 Uiso 1 1 calc R . .
C29 C 0.9794(10) 1.0716(10) 0.4046(8) 0.028(3) Uani 1 1 d . . .
C30 C 1.0824(9) 1.0241(10) 0.4065(8) 0.022(3) Uani 1 1 d . . .
C31 C 1.1863(10) 1.1052(10) 0.4671(8) 0.032(3) Uani 1 1 d . . .
H31 H 1.2571 1.0757 0.4720 0.038 Uiso 1 1 calc R . .
C32 C 1.1897(10) 1.2259(11) 0.5199(9) 0.037(3) Uani 1 1 d . . .
H32 H 1.2619 1.2811 0.5576 0.044 Uiso 1 1 calc R . .
C33 C 1.0835(12) 1.2651(11) 0.5163(9) 0.038(3) Uani 1 1 d . . .
H33 H 1.0844 1.3486 0.5562 0.046 Uiso 1 1 calc R . .
C34 C 0.6854(9) 1.3667(9) 0.3738(8) 0.028(3) Uani 1 1 d . . .
C35 C 0.5772(9) 1.4010(10) 0.3535(9) 0.032(3) Uani 1 1 d . . .
C36 C 0.4862(10) 1.3677(10) 0.3944(9) 0.033(3) Uani 1 1 d . . .
H36 H 0.4123 1.3896 0.3828 0.039 Uiso 1 1 calc R . .
C37 C 0.5028(11) 1.3050(11) 0.4500(10) 0.042(3) Uani 1 1 d . . .
H37 H 0.4409 1.2826 0.4777 0.051 Uiso 1 1 calc R . .
C38 C 0.6090(12) 1.2734(10) 0.4665(9) 0.040(3) Uani 1 1 d . . .
H38 H 0.6178 1.2273 0.5045 0.048 Uiso 1 1 calc R . .
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'
P P 0.1023 0.0942 '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'
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
N3 Cu1 N2 172.9(4) . . ?
N6 Cu2 N5 114.2(4) . . ?
N6 Cu2 N4 106.1(4) . . ?
N5 Cu2 N4 110.7(4) . . ?
N6 Cu2 N1 105.4(4) . . ?
N5 Cu2 N1 101.9(4) . . ?
N4 Cu2 N1 118.7(3) . . ?
F6 P1 F1 166.2(7) . . ?
F6 P1 F3 96.0(6) . . ?
F1 P1 F3 97.1(6) . . ?
F6 P1 F2 95.0(6) . . ?
F1 P1 F2 88.9(6) . . ?
F3 P1 F2 92.1(4) . . ?
F6 P1 F5 87.7(6) . . ?
F1 P1 F5 87.9(6) . . ?
F3 P1 F5 90.4(4) . . ?
F2 P1 F5 176.1(6) . . ?
F6 P1 F4 82.4(7) . . ?
F1 P1 F4 84.6(7) . . ?
F3 P1 F4 177.7(6) . . ?
F2 P1 F4 86.3(5) . . ?
F5 P1 F4 91.3(5) . . ?
F7 P2 F12 165.2(8) . . ?
F7 P2 F8 94.8(7) . . ?
F12 P2 F8 95.9(6) . . ?
F7 P2 F9 94.8(6) . . ?
F12 P2 F9 94.7(5) . . ?
F8 P2 F9 93.5(5) . . ?
F7 P2 F11 85.3(7) . . ?
F12 P2 F11 83.7(6) . . ?
F8 P2 F11 178.4(6) . . ?
F9 P2 F11 88.1(5) . . ?
F7 P2 F10 82.8(6) . . ?
F12 P2 F10 87.5(6) . . ?
F8 P2 F10 87.8(5) . . ?
F9 P2 F10 177.4(6) . . ?
F11 P2 F10 90.6(6) . . ?
C15 N1 C19 117.5(10) . . ?
C15 N1 Cu2 117.7(8) . . ?
C19 N1 Cu2 124.8(7) . . ?
C33 N2 C29 118.1(10) . . ?
C33 N2 Cu1 120.2(8) . . ?
C29 N2 Cu1 121.7(8) . . ?
C38 N3 C34 116.9(10) . . ?
C38 N3 Cu1 121.6(8) . . ?
C34 N3 Cu1 121.4(8) . . ?
C22 N4 C26 116.2(9) . . ?
C22 N4 Cu2 119.3(8) . . ?
C26 N4 Cu2 124.1(7) . . ?
C8 N5 Cu2 168.8(10) . . ?
C7 N6 Cu2 166.7(10) . . ?
C2 C1 C6 121.2(11) . . ?
C2 C1 C7 119.7(11) . . ?
C6 C1 C7 119.0(11) . . ?
C3 C2 C1 119.1(11) . . ?
C2 C3 C4 119.7(12) . . ?
C5 C4 C3 121.1(11) . . ?
C4 C5 C6 119.7(12) . . ?
C5 C6 C1 119.1(11) . . ?
N6 C7 C1 178.4(13) . . ?
N5 C8 C9 176.8(12) . . ?
C14 C9 C10 118.7(10) . . ?
C14 C9 C8 120.9(11) . . ?
C10 C9 C8 120.3(11) . . ?
C11 C10 C9 119.8(11) . . ?
C10 C11 C12 121.1(12) . . ?
C11 C12 C13 120.5(11) . . ?
C12 C13 C14 119.4(12) . . ?
C9 C14 C13 120.4(11) . . ?
N1 C15 C16 124.7(11) . . ?
C17 C16 C15 117.8(11) . . ?
C16 C17 C18 120.7(12) . . ?
C17 C18 C19 118.0(11) . . ?
C17 C18 C35 122.6(11) . 1_545 ?
C19 C18 C35 119.3(10) . 1_545 ?
N1 C19 C20 117.9(10) . . ?
N1 C19 C18 121.3(10) . . ?
C20 C19 C18 120.8(10) . . ?
C21 C20 C19 120.5(10) . . ?
C20 C21 C34 120.5(10) . 1_545 ?
N4 C22 C23 125.3(11) . . ?
C24 C23 C22 117.6(10) . . ?
C23 C24 C25 121.2(10) . . ?
C24 C25 C26 116.8(10) . . ?
C24 C25 C30 122.6(10) . . ?
C26 C25 C30 120.6(10) . . ?
N4 C26 C25 122.8(9) . . ?
N4 C26 C27 119.0(9) . . ?
C25 C26 C27 118.1(10) . . ?
C28 C27 C26 122.5(10) . . ?
C27 C28 C29 119.5(10) . . ?
N2 C29 C30 121.9(10) . . ?
N2 C29 C28 116.7(10) . . ?
C30 C29 C28 121.4(10) . . ?
C31 C30 C29 117.0(10) . . ?
C31 C30 C25 125.3(10) . . ?
C29 C30 C25 117.8(10) . . ?
C32 C31 C30 121.9(11) . . ?
C31 C32 C33 117.5(11) . . ?
N2 C33 C32 123.7(11) . . ?
N3 C34 C35 121.8(10) . . ?
N3 C34 C21 117.9(10) . 1_565 ?
C35 C34 C21 120.3(11) . 1_565 ?
C36 C35 C34 117.4(11) . . ?
C36 C35 C18 124.2(10) . 1_565 ?
C34 C35 C18 118.4(10) . 1_565 ?
C37 C36 C35 120.3(11) . . ?
C36 C37 C38 119.8(12) . . ?
N3 C38 C37 123.7(11) . . ?
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 N3 1.859(9) . ?
Cu1 N2 1.877(9) . ?
Cu2 N6 2.001(11) . ?
Cu2 N5 2.006(11) . ?
Cu2 N4 2.083(9) . ?
Cu2 N1 2.099(9) . ?
P1 F6 1.517(9) . ?
P1 F1 1.551(10) . ?
P1 F3 1.575(7) . ?
P1 F2 1.576(8) . ?
P1 F5 1.591(8) . ?
P1 F4 1.605(10) . ?
P2 F7 1.489(9) . ?
P2 F12 1.528(10) . ?
P2 F8 1.533(8) . ?
P2 F9 1.554(8) . ?
P2 F11 1.568(10) . ?
P2 F10 1.603(9) . ?
N1 C15 1.334(14) . ?
N1 C19 1.372(13) . ?
N2 C33 1.329(14) . ?
N2 C29 1.371(13) . ?
N3 C38 1.349(15) . ?
N3 C34 1.372(14) . ?
N4 C22 1.319(13) . ?
N4 C26 1.358(13) . ?
N5 C8 1.157(14) . ?
N6 C7 1.151(14) . ?
C1 C2 1.377(16) . ?
C1 C6 1.387(16) . ?
C1 C7 1.468(18) . ?
C2 C3 1.377(15) . ?
C3 C4 1.384(17) . ?
C4 C5 1.366(17) . ?
C5 C6 1.381(16) . ?
C8 C9 1.438(17) . ?
C9 C14 1.374(15) . ?
C9 C10 1.404(16) . ?
C10 C11 1.354(16) . ?
C11 C12 1.355(16) . ?
C12 C13 1.369(16) . ?
C13 C14 1.386(15) . ?
C15 C16 1.390(16) . ?
C16 C17 1.353(16) . ?
C17 C18 1.406(15) . ?
C18 C19 1.409(15) . ?
C18 C35 1.439(15) 1_545 ?
C19 C20 1.402(14) . ?
C20 C21 1.362(14) . ?
C21 C34 1.428(14) 1_545 ?
C22 C23 1.388(15) . ?
C23 C24 1.340(15) . ?
C24 C25 1.393(14) . ?
C25 C26 1.408(14) . ?
C25 C30 1.446(14) . ?
C26 C27 1.427(14) . ?
C27 C28 1.355(14) . ?
C28 C29 1.418(15) . ?
C29 C30 1.407(14) . ?
C30 C31 1.388(15) . ?
C31 C32 1.363(15) . ?
C32 C33 1.391(16) . ?
C34 C35 1.413(15) . ?
C34 C21 1.428(14) 1_565 ?
C35 C36 1.400(15) . ?
C35 C18 1.439(15) 1_565 ?
C36 C37 1.342(16) . ?
C37 C38 1.364(16) . ?
