#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/16/2011632.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2011632
loop_
_publ_author_name
'Kim, Jun Hwan'
'Roh, Soo-Gyun'
'Jeong, Jong Hwa'
_publ_section_title
;Di-μ-methoxo-bis({N,N'-bis[2-(3,5-dimethylpyrazol-1-yl)ethyl]amine-κ³N}copper(II))
 bis(hexafluorophosphate)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e543
_journal_page_last               e544
_journal_paper_doi               10.1107/S0108270100014815
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Cu2 (C14 H23 N5)2 (C H3 O)2] (P F6)2'
_chemical_formula_moiety         'C30 H52 Cu2 N10 O2 2+, 2P2 F6 1-'
_chemical_formula_sum            'C30 H52 Cu2 F12 N10 O2 P2'
_chemical_formula_weight         1001.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1607(7)
_cell_length_b                   12.7860(9)
_cell_length_c                   23.3160(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      9.8
_cell_volume                     4519.7(4)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD (McArdle, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .995
_diffrn_measured_fraction_theta_max .995
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0071
_diffrn_reflns_av_sigmaI/netI    .1092
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4256
_diffrn_reflns_theta_full        25.47
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        .2
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal rod'
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .30
_refine_diff_density_max         .984
_refine_diff_density_min         -.526
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.380
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.380
_refine_ls_R_factor_all          .149
_refine_ls_R_factor_gt           .069
_refine_ls_shift/su_max          .014
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0720P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .189
_reflns_number_gt                2065
_reflns_number_total             4174
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0421.cif
_cod_data_source_block           I
_cod_database_code               2011632
_cod_database_fobs_code          2011632
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu .03778(4) .92866(6) .04655(3) .0399(2) Uani d . 1 . . Cu
N1 .1639(3) .9138(4) .0742(2) .0477(14) Uani d . 1 . . N
C1 .2382(4) .9068(5) .0430(3) .0501(16) Uani d . 1 . . C
C2 .3097(4) .8942(6) .0806(3) .063(2) Uani d . 1 A . C
H2 .3685 .8860 .0702 .076 Uiso calc R 1 . . H
C3 .2778(5) .8962(8) .1338(4) .088(3) Uani d . 1 . . C
N2 .1886(4) .9059(5) .1296(2) .0627(18) Uani d . 1 A . N
C4 .1253(5) .9149(7) .1754(3) .072(3) Uani d . 1 . . C
H4A .1563 .9130 .2118 .086 Uiso calc R 1 A . H
H4B .0861 .8549 .1742 .086 Uiso calc R 1 . . H
C5 .0699(5) 1.0150(7) .1727(3) .067(2) Uani d . 1 A . C
H5A .0486 1.0327 .2107 .080 Uiso calc R 1 . . H
H5B .1059 1.0725 .1589 .080 Uiso calc R 1 . . H
N3 -.0056(4) .9989(5) .1337(2) .0525(14) Uani d . 1 . . N
H3N -.0259 1.0642 .1254 .063 Uiso calc R 1 A . H
C6 -.0791(5) .9457(6) .1622(3) .065(2) Uani d . 1 A . C
H6A -.1213 .9976 .1752 .078 Uiso calc R 1 . . H
H6B -.0570 .9093 .1958 .078 Uiso calc R 1 . . H
C7 -.1253(5) .8691(6) .1245(4) .064(2) Uani d . 1 . . C
H7A -.1787 .8451 .1433 .077 Uiso calc R 1 A . H
H7B -.1422 .9033 .0890 .077 Uiso calc R 1 . . H
N4 -.0683(4) .7778(4) .1113(2) .0496(14) Uani d . 1 A . N
N5 .0011(4) .7877(4) .0739(2) .0496(14) Uani d . 1 . . N
C8 .0350(5) .6926(5) .0689(3) .0560(18) Uani d . 1 A . C
C9 -.0118(5) .6230(6) .1020(3) .073(2) Uani d . 1 . . C
H9 -.0010 .5517 .1054 .087 Uiso calc R 1 A . H
C10 -.0774(5) .6786(5) .1290(3) .0569(19) Uani d . 1 A . C
C11 .2385(5) .9125(6) -.0195(3) .068(2) Uani d . 1 . . C
H11A .1792 .9068 -.0335 .102 Uiso calc R 1 . . H
H11B .2734 .8563 -.0347 .102 Uiso calc R 1 . . H
H11C .2632 .9781 -.0314 .102 Uiso calc R 1 . . H
C12a .3222(13) .8440(16) .1890(8) .088(6) Uiso d P .50 A 1 C
H12A .2910 .8656 .2228 .133 Uiso calc PR .50 A 1 H
H12B .3826 .8659 .1917 .133 Uiso calc PR .50 A 1 H
H12C .3196 .7693 .1856 .133 Uiso calc PR .50 A 1 H
C12b .3247(11) .9113(14) .1905(7) .070(4) Uiso d P .50 A 2 C
H12D .3261 .9843 .1999 .105 Uiso calc PR .50 A 2 H
H12E .3839 .8852 .1875 .105 Uiso calc PR .50 A 2 H
H12F .2938 .8738 .2200 .105 Uiso calc PR .50 A 2 H
C13 .1110(6) .6712(7) .0304(4) .083(3) Uani d . 1 . . C
H13A .1030 .7079 -.0051 .124 Uiso calc R 1 A . H
H13B .1146 .5974 .0231 .124 Uiso calc R 1 . . H
H13C .1644 .6943 .0485 .124 Uiso calc R 1 . . H
C14 -.1455(6) .6437(7) .1705(4) .089(3) Uani d . 1 . . C
H14A -.1355 .6767 .2068 .134 Uiso calc R 1 A . H
H14B -.1423 .5691 .1749 .134 Uiso calc R 1 . . H
H14C -.2029 .6626 .1564 .134 Uiso calc R 1 . . H
O1 .0596(2) 1.0599(3) .00707(17) .0421(10) Uani d . 1 . . O
C15 .1108(4) 1.1426(6) .0301(3) .057(2) Uani d . 1 A . C
H15A .0744 1.1854 .0543 .086 Uiso calc R 1 . . H
H15B .1342 1.1842 -.0006 .086 Uiso calc R 1 . . H
H15C .1585 1.1141 .0523 .086 Uiso calc R 1 . . H
P .09211(14) .80109(18) .33879(10) .0675(6) Uani d . 1 . . P
F1A .0437(10) .8742(12) .2916(6) .123(5) Uiso d P .50 . . F
F1B .0569(6) .9041(8) .3097(4) .066(3) Uiso d P .50 . . F
F2A .1416(11) .6978(13) .3595(7) .136(6) Uiso d P .50 . . F
F2B .1226(8) .7121(9) .3820(5) .085(4) Uiso d P .50 . . F
F3A .1057(14) .8849(15) .3861(8) .175(7) Uiso d P .50 . . F
F3B .1564(8) .8648(10) .3795(5) .095(4) Uiso d P .50 . . F
F4A .1706(8) .7851(10) .2957(5) .097(3) Uiso d P .50 . . F
F4B .1809(7) .8423(9) .3088(5) .093(3) Uiso d P .50 . . F
F5A .0205(7) .8350(9) .3867(4) .087(3) Uiso d P .50 . . F
F5B .0051(8) .7623(11) .3660(6) .112(4) Uiso d P .50 . . F
F6A .0176(10) .7321(11) .3120(6) .127(4) Uiso d P .50 . . F
F6B .0697(9) .7255(10) .2851(5) .116(4) Uiso d P .50 . . F
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Cu O1 5_575 . 76.06(18)
O1 Cu N5 5_575 . 93.5(2)
O1 Cu N5 . . 168.9(2)
O1 Cu N1 5_575 . 158.46(19)
O1 Cu N1 . . 94.09(19)
N5 Cu N1 . . 94.4(2)
O1 Cu N3 5_575 . 108.66(19)
O1 Cu N3 . . 97.43(19)
N5 Cu N3 . . 89.5(2)
N1 Cu N3 . . 91.4(2)
O1 Cu Cu 5_575 5_575 38.05(12)
O1 Cu Cu . 5_575 38.01(11)
N5 Cu Cu . 5_575 131.49(17)
N1 Cu Cu . 5_575 129.45(16)
N3 Cu Cu . 5_575 106.56(14)
C1 N1 N2 . . 106.3(5)
C1 N1 Cu . . 128.6(4)
N2 N1 Cu . . 125.1(4)
N1 C1 C2 . . 108.4(6)
N1 C1 C11 . . 122.8(6)
C2 C1 C11 . . 128.8(6)
C3 C2 C1 . . 107.5(6)
C2 C3 N2 . . 107.1(7)
C2 C3 C12b . . 130.2(9)
N2 C3 C12b . . 121.3(9)
C2 C3 C12a . . 126.1(10)
N2 C3 C12a . . 121.0(10)
C12a C3 C12b . . 32.0(8)
N1 N2 C3 . . 110.7(6)
N1 N2 C4 . . 121.2(5)
C3 N2 C4 . . 127.9(6)
N2 C4 C5 . . 113.6(6)
N3 C5 C4 . . 109.5(6)
C6 N3 C5 . . 112.1(6)
C6 N3 Cu . . 115.7(4)
C5 N3 Cu . . 112.0(4)
N3 C6 C7 . . 113.2(6)
N4 C7 C6 . . 111.4(6)
C10 N4 N5 . . 111.2(5)
C10 N4 C7 . . 128.3(6)
N5 N4 C7 . . 120.4(5)
C8 N5 N4 . . 105.6(5)
C8 N5 Cu . . 133.9(5)
N4 N5 Cu . . 120.1(4)
N5 C8 C9 . . 110.1(6)
N5 C8 C13 . . 121.5(6)
C9 C8 C13 . . 128.3(7)
C8 C9 C10 . . 107.2(7)
N4 C10 C9 . . 105.8(6)
N4 C10 C14 . . 123.9(7)
C9 C10 C14 . . 130.3(7)
C15 O1 Cu . 5_575 127.2(4)
C15 O1 Cu . . 123.9(4)
Cu O1 Cu 5_575 . 103.94(18)
F5B P F3A . . 92.5(9)
F5B P F6A . . 50.7(6)
F3A P F6A . . 140.4(10)
F5B P F4A . . 150.1(7)
F3A P F4A . . 116.3(9)
F6A P F4A . . 102.6(7)
F5B P F1B . . 99.0(6)
F3A P F1B . . 76.9(8)
F6A P F1B . . 93.2(6)
F4A P F1B . . 95.2(6)
F5B P F3B . . 116.4(7)
F3A P F3B . . 30.4(7)
F6A P F3B . . 166.7(7)
F4A P F3B . . 89.1(6)
F1B P F3B . . 92.1(6)
F5B P F2B . . 76.0(6)
F3A P F2B . . 90.3(8)
F6A P F2B . . 93.4(7)
F4A P F2B . . 95.3(6)
F1B P F2B . . 166.1(6)
F3B P F2B . . 79.0(6)
F5B P F2A . . 90.6(8)
F3A P F2A . . 107.1(9)
F6A P F2A . . 89.6(8)
F4A P F2A . . 74.3(7)
F1B P F2A . . 169.5(7)
F3B P F2A . . 87.4(7)
F2B P F2A . . 22.7(6)
F5B P F4B . . 178.3(6)
F3A P F4B . . 88.3(9)
F6A P F4B . . 128.1(7)
F4A P F4B . . 29.4(5)
F1B P F4B . . 79.8(5)
F3B P F4B . . 64.9(6)
F2B P F4B . . 105.5(6)
F2A P F4B . . 90.5(7)
F5B P F5A . . 39.6(5)
F3A P F5A . . 54.0(8)
F6A P F5A . . 86.7(7)
F4A P F5A . . 170.2(6)
F1B P F5A . . 81.1(5)
F3B P F5A . . 82.0(6)
F2B P F5A . . 87.1(6)
F2A P F5A . . 109.2(7)
F4B P F5A . . 140.8(6)
F5B P F6B . . 86.9(7)
F3A P F6B . . 172.2(9)
F6A P F6B . . 37.1(6)
F4A P F6B . . 65.6(6)
F1B P F6B . . 95.5(6)
F3B P F6B . . 154.0(7)
F2B P F6B . . 97.1(6)
F2A P F6B . . 80.7(7)
F4B P F6B . . 92.0(6)
F5A P F6B . . 123.7(7)
F5B P F1A . . 94.4(7)
F3A P F1A . . 98.3(9)
F6A P F1A . . 74.1(7)
F4A P F1A . . 89.1(6)
F1B P F1A . . 21.8(6)
F3B P F1A . . 112.9(7)
F2B P F1A . . 167.5(7)
F2A P F1A . . 153.8(8)
F4B P F1A . . 84.0(7)
F5A P F1A . . 90.6(6)
F6B P F1A . . 74.0(7)
F1B F1A P . . 75(2)
F1A F1B P . . 83(2)
F2B F2A P . . 78(2)
F2A F2B P . . 79(2)
F3B F3A F5A . . 134(2)
F3B F3A P . . 77.1(18)
F5A F3A P . . 65.3(10)
F3A F3B P . . 72.5(17)
F3A F3B F4B . . 115.7(19)
P F3B F4B . . 58.1(5)
F4B F4A P . . 77.7(13)
F4B F4A F6B . . 128.8(16)
P F4A F6B . . 58.6(6)
F4A F4B P . . 72.8(13)
F4A F4B F3B . . 118.3(15)
P F4B F3B . . 57.0(5)
F5B F5A F3A . . 125.0(14)
F5B F5A P . . 66.6(9)
F3A F5A P . . 60.6(9)
F5A F5B F6A . . 130.3(15)
F5A F5B P . . 73.8(9)
F6A F5B P . . 65.4(9)
F6B F6A F5B . . 136.2(17)
F6B F6A P . . 74.4(12)
F5B F6A P . . 64.0(8)
F6A F6B P . . 68.5(12)
F6A F6B F4A . . 124.3(15)
P F6B F4A . . 55.9(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu O1 5_575 1.940(4) ?
Cu O1 . 1.942(4) ?
Cu N5 . 1.991(5) ?
Cu N1 . 2.026(5) ?
Cu N3 . 2.317(5) ?
Cu Cu 5_575 3.0582(14) ?
N1 C1 . 1.345(8) ?
N1 N2 . 1.347(7) ?
C1 C2 . 1.404(9) ?
C1 C11 . 1.458(9) ?
C2 C3 . 1.333(10) ?
C3 N2 . 1.361(9) ?
C3 C12b . 1.512(18) ?
C3 C12a . 1.597(19) ?
N2 C4 . 1.442(8) ?
C4 C5 . 1.533(11) ?
C5 N3 . 1.475(9) ?
N3 C6 . 1.466(9) ?
C6 C7 . 1.492(10) ?
C7 N4 . 1.484(9) ?
N4 C10 . 1.342(8) ?
N4 N5 . 1.372(7) ?
N5 C8 . 1.326(8) ?
C8 C9 . 1.374(10) ?
C8 C13 . 1.485(10) ?
C9 C10 . 1.376(10) ?
C10 C14 . 1.483(9) ?
O1 C15 . 1.418(7) ?
O1 Cu 5_575 1.940(4) ?
P F5B . 1.545(12) ?
P F3A . 1.551(19) ?
P F6A . 1.563(14) ?
P F4A . 1.570(11) ?
P F1B . 1.574(10) ?
P F3B . 1.585(12) ?
P F2B . 1.590(12) ?
P F2A . 1.594(16) ?
P F4B . 1.605(11) ?
P F5A . 1.617(10) ?
P F6B . 1.618(13) ?
P F1A . 1.620(15) ?
F1A F1B . .605(17) ?
F2A F2B . .626(18) ?
F3A F3B . .82(2) ?
F3A F5A . 1.441(19) ?
F3B F4B . 1.713(15) ?
F4A F4B . .808(13) ?
F4A F6B . 1.727(17) ?
F5A F5B . 1.074(14) ?
F5B F6A . 1.330(16) ?
F6A F6B . 1.013(15) ?
