#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/94/4319471.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_4319471
loop_
_publ_author_name
'Bim Graham'
'Milton T. W. Hearn'
'Peter C. Junk'
'Christopher M. Kepert'
'Frank E. Mabbs'
'Boujemaa Moubaraki'
'Keith S. Murray'
'Leone Spiccia'
_publ_section_title
;
 Syntheses, Crystal Structures, Magnetic Properties, and EPR Spectra of
 Tetranuclear Copper(II) Complexes Featuring Pairs of "Roof-Shaped" Cu2X2
 Dimers with Hydroxide, Methoxide, and Azide Bridges
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1536
_journal_page_last               1543
_journal_paper_doi               10.1021/ic000991h
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural     C46H92N30Cu4F24O4P4
_chemical_formula_sum            'C23 H46 Cu2 F12 N15 O2 P2'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             98-08-21
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                91.846(11)
_cell_angle_beta                 98.218(12)
_cell_angle_gamma                105.617(17)
_cell_formula_units_Z            2
_cell_length_a                   12.060(2)
_cell_length_b                   12.554(2)
_cell_length_c                   14.0509(15)
_cell_measurement_temperature    293
_cell_volume                     2022.2(5)
_computing_data_reduction        xtal_DIFDAT_SORTRF_ADDREF_ABSORB
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal
_diffrn_ambient_temperature      296
_diffrn_measurement_device       CAD4
_diffrn_radiation_source         MoKa
_diffrn_radiation_type           xray_tube
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .036
_diffrn_reflns_av_sigmaI/netI    .092
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7127
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.47
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.23
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.438
_refine_diff_density_min         -2.95
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.579
_refine_ls_goodness_of_fit_obs   2.169
_refine_ls_matrix_type           atomblock
_refine_ls_number_constraints    0
_refine_ls_number_parameters     506
_refine_ls_number_reflns         3129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .202
_refine_ls_R_factor_obs          .068
_refine_ls_shift/esd_max         .238
_refine_ls_shift/esd_mean        .05
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .078
_refine_ls_wR_factor_obs         .069
_reflns_d_resolution_high        .842
_reflns_d_resolution_low         13.868
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_observed          3129
_reflns_number_total             7110
_reflns_observed_criterion       refl_observed_if_F____>_.000_sigma(F___)
_cod_data_source_file            ic000991h_3.cif
_cod_data_source_block           '[Cu4Ldur(mu2-N3)4](PF6)4.4H2O.6CH3CN'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2022.1(6)
_cod_original_sg_symbol_Hall     -p_1
_cod_original_formula_sum        'C23 H46 N15 Cu2 F12 O2 P2'
_cod_database_code               4319471
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_a_min  1.088
_exptl_absorpt_correction_a_max  1.241
#END Tags that were not found in dictionaries
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
_atom_site_calc_attached_atom
Cu1 .24309(12) .27739(12) 1.20118(10) .0337(7) Uani ? ?
Cu2 -.00489(13) -.21890(12) .74051(10) .0333(7) Uani ? ?
N1 .1495(7) -.0652(7) .7908(6) .033(5) Uani ? ?
N2 .1172(8) -.3037(7) .7641(6) .040(5) Uani ? ?
N3 .0438(9) -.1929(7) .6101(6) .043(5) Uani ? ?
C1 .2239(10) -.1193(10) .8534(8) .040(6) Uani ? ?
C2 .2317(10) -.2275(10) .8066(8) .042(6) Uani ? ?
C3 .1153(11) -.3532(10) .6642(8) .050(7) Uani ? ?
C4 .1247(11) -.2660(10) .5933(8) .051(7) Uani ? ?
C5 .1012(11) -.0753(10) .6136(8) .050(7) Uani ? ?
C6 .1980(10) -.0340(9) .7020(8) .042(6) Uani ? ?
N4 .3101(7) .1784(7) 1.0927(6) .037(5) Uani ? ?
N5 .3179(8) .4087(7) 1.1340(6) .040(5) Uani ? ?
N6 .4035(8) .3002(8) 1.2781(6) .043(5) Uani ? ?
C7 .3070(10) .2520(9) 1.0122(8) .035(6) Uani ? ?
C8 .3613(10) .3736(10) 1.0428(8) .040(6) Uani ? ?
C9 .4143(11) .4811(9) 1.2040(8) .047(7) Uani ? ?
C10 .4822(11) .4089(11) 1.2579(8) .055(7) Uani ? ?
C11 .4399(10) .2012(10) 1.2479(9) .048(7) Uani ? ?
C12 .4306(9) .1862(9) 1.1398(9) .041(6) Uani ? ?
C13 .1382(10) .0394(9) .8406(8) .039(6) Uani ? ?
C14 .0719(9) .0172(8) .9268(8) .032(6) Uani ? ?
C15 -.0501(10) -.0154(8) .9077(7) .034(6) Uani ? ?
C16 .1232(9) .0324(8) 1.0244(8) .030(6) Uani ? ?
C17 .2535(9) .0598(9) 1.0572(8) .034(6) Uani ? ?
N7 .1573(8) .1786(8) 1.2921(6) .038(5) Uani ? ?
N8 .1949(9) .1513(8) 1.3680(7) .053(6) Uani ? ?
N9 .2289(11) .1259(11) 1.4402(8) .096(9) Uani ? ?
N10 .0782(7) .2725(7) 1.1468(6) .033(5) Uani ? ?
N11 .0384(8) .2750(7) 1.0641(6) .035(5) Uani ? ?
N12 .0006(10) .2777(10) .9862(7) .066(7) Uani ? ?
P1 .5795(3) .1887(3) .8748(3) .052(2) Uani ? ?
P2 .2484(4) .4863(3) 1.4459(3) .074(3) Uani ? ?
F1 .5877(8) .0890(6) .8063(6) .084(5) Uani ? ?
F2 .7096(7) .2043(8) .9236(6) .100(6) Uani ? ?
F3 .6271(8) .2740(7) .7995(6) .089(5) Uani ? ?
F4 .5760(7) .2898(7) .9433(6) .087(5) Uani ? ?
F5 .4496(7) .1742(8) .8262(7) .115(7) Uani ? ?
F6 .5343(9) .1065(7) .9510(6) .103(6) Uani ? ?
F7 .1941(8) .4382(7) 1.3374(6) .101(6) Uani ? ?
F8 .1620(12) .5568(10) 1.4431(8) .180(10) Uani ? ?
F9 .1586(8) .3872(9) 1.4812(7) .127(7) Uani ? ?
F10 .3007(8) .5307(9) 1.5535(6) .118(6) Uani ? ?
F11 .3355(9) .4135(9) 1.4468(7) .127(7) Uani ? ?
F12 .3388(11) .5790(9) 1.4069(8) .165(9) Uani ? ?
N1s .2197(15) .3984(15) .7976(10) .143(12) Uani ? ?
C1s .2512(14) .3514(13) .7405(11) .092(10) Uani ? ?
C2s .2981(15) .2971(13) .6698(10) .088(10) Uani ? ?
N2s -.0065(13) .1660(12) .6261(9) .111(10) Uani ? ?
C3s -.0647(16) .1934(14) .6727(10) .101(11) Uani ? ?
C4s -.1336(18) .241(2) .7301(12) .149(16) Uani ? ?
N3s .6011(13) .1186(14) 1.4402(11) .136(12) Uani ? ?
C5s .5587(15) .1451(17) 1.5042(12) .122(13) Uani ? ?
C6s .5039(16) .1677(18) 1.5780(12) .128(13) Uani ? ?
O1s .1585(8) .5470(7) 1.0810(6) .067(5) Uani ? ?
O2s .0719(9) .5139(8) .8832(6) .075(6) Uani ? ?
H1a .30868 -.06350 .87053 .03500 Uiso ? ?
H1b .19072 -.13504 .91748 .03500 Uiso ? ?
H2a .28477 -.20935 .75145 .03500 Uiso ? ?
H2b .27484 -.26880 .85793 .03500 Uiso ? ?
H3a .03680 -.41603 .64341 .03500 Uiso ? ?
H3b .18412 -.39057 .66481 .03500 Uiso ? ?
H4a .10335 -.30133 .52205 .03500 Uiso ? ?
H4b .21257 -.21534 .60157 .03500 Uiso ? ?
H5a .03866 -.03035 .61712 .03500 Uiso ? ?
H5b .13605 -.05584 .54958 .03500 Uiso ? ?
H6a .23526 .05230 .70452 .03500 Uiso ? ?
H6b .26670 -.07129 .69555 .03500 Uiso ? ?
H7a .35097 .22963 .95887 .03500 Uiso ? ?
H7b .22005 .24208 .98103 .03500 Uiso ? ?
H8a .45143 .38862 1.05735 .03500 Uiso ? ?
H8b .33971 .42027 .98694 .03500 Uiso ? ?
H9a .46995 .54184 1.16829 .03500 Uiso ? ?
H9b .38113 .52338 1.25348 .03500 Uiso ? ?
H10a .54391 .39477 1.21441 .03500 Uiso ? ?
H10b .53155 .45244 1.32203 .03500 Uiso ? ?
H11a .52701 .21033 1.28093 .03500 Uiso ? ?
H11b .38740 .12992 1.27169 .03500 Uiso ? ?
H12a .49108 .25550 1.11548 .03500 Uiso ? ?
H12b .45515 .11547 1.11950 .03500 Uiso ? ?
H15 -.09007 -.02734 .83415 .03500 Uiso ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 34 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
H ? 0 66 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
N ? 0 24 .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
Cu ? 0 4 .263 1.266 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
P ? 0 4 .09 .095 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
F ? 0 24 .014 .01 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
O ? 0 4 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Cu1 N6 85.1(4) . . . ?
N5 Cu1 N7 163.5(4) . . . ?
N5 Cu1 N10 95.8(4) . . . ?
N6 Cu1 N7 95.8(4) . . . ?
N6 Cu1 N10 168.6(4) . . . ?
N7 Cu1 N10 80.1(4) . . . ?
N2 Cu2 N3 86.6(4) . . . ?
N2 Cu2 N7 163.6(3) . . 2 ?
N2 Cu2 N10 93.9(4) . . 2 ?
N3 Cu2 N7 95.6(4) . . 2 ?
N3 Cu2 N10 167.5(3) . . 2 ?
N7 Cu2 N10 80.4(4) 2 . 2 ?
C1 N1 C6 110.9(9) . . . ?
C1 N1 C13 111.9(8) . . . ?
C6 N1 C13 107.5(8) . . . ?
Cu2 N2 C2 110.3(7) . . . ?
Cu2 N2 C3 102.3(7) . . . ?
C2 N2 C3 113.5(9) . . . ?
Cu2 N3 C4 108.6(7) . . . ?
Cu2 N3 C5 105.3(7) . . . ?
C4 N3 C5 113.1(10) . . . ?
N1 C1 C2 112.8(9) . . . ?
N2 C2 C1 113.9(10) . . . ?
N2 C3 C4 110.5(10) . . . ?
N3 C4 C3 110.1(10) . . . ?
N3 C5 C6 113.2(10) . . . ?
N1 C6 C5 109.4(9) . . . ?
C7 N4 C12 112.6(8) . . . ?
C7 N4 C17 110.6(8) . . . ?
C12 N4 C17 107.4(9) . . . ?
Cu1 N5 C8 111.3(7) . . . ?
Cu1 N5 C9 107.5(7) . . . ?
C8 N5 C9 111.9(9) . . . ?
Cu1 N6 C10 109.7(7) . . . ?
Cu1 N6 C11 104.3(6) . . . ?
C10 N6 C11 114.2(10) . . . ?
N4 C7 C8 113.7(8) . . . ?
N5 C8 C7 111.7(9) . . . ?
N5 C9 C10 108.6(9) . . . ?
N6 C10 C9 111.9(9) . . . ?
N6 C11 C12 111.8(10) . . . ?
N4 C12 C11 110.3(10) . . . ?
N1 C13 C14 113.2(8) . . . ?
C13 C14 C15 117.8(9) . . . ?
C13 C14 C16 125.5(9) . . . ?
C15 C14 C16 116.6(10) . . . ?
C14 C15 C16 125.8(9) . . 2 ?
C14 C16 C17 123.2(10) . . . ?
C14 C16 C15 117.6(10) . . 2 ?
C17 C16 C15 119.1(9) . . 2 ?
N4 C17 C16 114.4(10) . . . ?
Cu1 N7 N8 128.9(8) . . . ?
Cu1 N7 Cu2 96.2(4) . . 2 ?
N8 N7 Cu2 126.4(9) . . 2 ?
N7 N8 N9 178.9(15) . . . ?
Cu1 N10 N11 127.5(8) . . . ?
Cu1 N10 Cu2 98.0(4) . . 2 ?
N11 N10 Cu2 132.1(7) . . 2 ?
N10 N11 N12 179.6(13) . . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N5 1.992(9) . . ?
Cu1 N6 2.019(9) . . ?
Cu1 N7 2.008(9) . . ?
Cu1 N10 2.010(9) . . ?
Cu2 N2 2.034(11) . . ?
Cu2 N3 2.013(9) . . ?
Cu2 N7 2.030(10) . 2 ?
Cu2 N10 1.972(9) . 2 ?
N1 C1 1.478(15) . . ?
N1 C6 1.474(15) . . ?
N1 C13 1.515(15) . . ?
N2 C2 1.482(13) . . ?
N2 C3 1.511(15) . . ?
N3 C4 1.545(18) . . ?
N3 C5 1.448(14) . . ?
C1 C2 1.521(18) . . ?
C3 C4 1.496(17) . . ?
C5 C6 1.547(15) . . ?
N4 C7 1.486(14) . . ?
N4 C12 1.484(14) . . ?
N4 C17 1.496(13) . . ?
N5 C8 1.545(15) . . ?
N5 C9 1.480(13) . . ?
N6 C10 1.500(15) . . ?
N6 C11 1.493(17) . . ?
C7 C8 1.511(15) . . ?
C9 C10 1.53(2) . . ?
C11 C12 1.509(17) . . ?
C13 C14 1.538(16) . . ?
C14 C15 1.400(16) . . ?
C14 C16 1.405(14) . . ?
C15 C16 1.373(16) . 2 ?
C16 C17 1.514(15) . . ?
N7 N8 1.194(13) . . ?
N8 N9 1.127(16) . . ?
N10 N11 1.197(11) . . ?
N11 N12 1.129(13) . . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
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
? ? ? ? ? ? ? ? ? ?
loop_
_reflns_scale_group_code
_reflns_scale_meas_F
? 6.1573
