#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:06:21 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178680 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/91/4079189.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_4079189
loop_
_publ_author_name
'Kirillov, Alexander M.'
'Filipowicz, Małgorzata'
'Guedes da Silva, M. Fátima C.'
'Kłak, Julia'
'Smoleński, Piotr'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Unprecedented Mixed-Valence Cu(I)/Cu(II) Complex Derived
 fromN-Methyl-1,3,5-triaza-7-phosphaadamantane: Synthesis, Structural
 Features, and Magnetic Properties
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              7921
_journal_paper_doi               10.1021/om3005564
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C28 H60 Cu4 I4 N30 P4, 2(H2 O)'
_chemical_formula_sum            'C28 H64 Cu4 I4 N30 O2 P4'
_chemical_formula_weight         1738.73
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                109.430(8)
_cell_angle_beta                 101.394(5)
_cell_angle_gamma                98.230(7)
_cell_formula_units_Z            1
_cell_length_a                   7.589(4)
_cell_length_b                   13.7459(12)
_cell_length_c                   14.8097(18)
_cell_measurement_reflns_used    5749
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.59
_cell_volume                     1391.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12877
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    3.903
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0294
_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)+(0.0331P)²+2.7680P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                4316
_reflns_number_total             5054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005564_si_002.cif
_cod_data_source_block           Piotr050810
_cod_original_cell_volume        1391.2(8)
_cod_database_code               4079189
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
C11 C 0.8111(5) 0.5442(3) 0.2667(3) 0.0139(8) Uani 1 1 d .
H11A H 0.8818 0.5987 0.2495 0.017 Uiso 1 1 calc R
H11B H 0.9008 0.5178 0.3055 0.017 Uiso 1 1 calc R
C12 C 0.4971(6) 0.6249(3) 0.2462(3) 0.0194(9) Uani 1 1 d .
H12A H 0.3935 0.6485 0.2720 0.023 Uiso 1 1 calc R
H12B H 0.5584 0.6811 0.2275 0.023 Uiso 1 1 calc R
C13 C 0.5324(6) 0.4822(3) 0.3439(3) 0.0176(9) Uani 1 1 d .
H13A H 0.6150 0.4526 0.3830 0.021 Uiso 1 1 calc R
H13B H 0.4320 0.4980 0.3763 0.021 Uiso 1 1 calc R
C14 C 0.5648(6) 0.4931(3) 0.1107(3) 0.0188(9) Uani 1 1 d .
H14A H 0.6321 0.5531 0.0989 0.023 Uiso 1 1 calc R
H14B H 0.5062 0.4355 0.0454 0.023 Uiso 1 1 calc R
C15 C 0.5917(6) 0.3666(3) 0.1957(3) 0.0150(9) Uani 1 1 d .
H15A H 0.5328 0.3050 0.1332 0.018 Uiso 1 1 calc R
H15B H 0.6769 0.3432 0.2397 0.018 Uiso 1 1 calc R
C16 C 0.3281(6) 0.4407(3) 0.1799(4) 0.0222(10) Uani 1 1 d .
H16A H 0.2633 0.3810 0.1168 0.027 Uiso 1 1 calc R
H16B H 0.2339 0.4659 0.2137 0.027 Uiso 1 1 calc R
C17 C 0.8300(6) 0.4077(3) 0.1145(3) 0.0226(10) Uani 1 1 d .
H17A H 0.7585 0.3489 0.0534 0.034 Uiso 1 1 calc R
H17B H 0.9164 0.3816 0.1542 0.034 Uiso 1 1 calc R
H17C H 0.8990 0.4622 0.0977 0.034 Uiso 1 1 calc R
C21 C 0.5731(5) 0.9374(3) 0.5882(3) 0.0118(8) Uani 1 1 d .
H21A H 0.6448 0.9917 0.5713 0.014 Uiso 1 1 calc R
H21B H 0.4608 0.9005 0.5328 0.014 Uiso 1 1 calc R
C22 C 0.5586(6) 0.7687(3) 0.6493(3) 0.0158(9) Uani 1 1 d .
H22A H 0.4453 0.7273 0.5959 0.019 Uiso 1 1 calc R
H22B H 0.6206 0.7182 0.6704 0.019 Uiso 1 1 calc R
C23 C 0.8802(5) 0.9270(3) 0.7183(3) 0.0115(8) Uani 1 1 d .
H23A H 0.9583 0.8843 0.7424 0.014 Uiso 1 1 calc R
H23B H 0.9615 0.9822 0.7068 0.014 Uiso 1 1 calc R
C24 C 0.3996(6) 0.9081(3) 0.7083(3) 0.0150(9) Uani 1 1 d .
H24A H 0.3514 0.9445 0.7649 0.018 Uiso 1 1 calc R
H24B H 0.2928 0.8659 0.6509 0.018 Uiso 1 1 calc R
C25 C 0.6678(6) 0.8997(3) 0.8168(3) 0.0147(9) Uani 1 1 d .
H25A H 0.7394 0.8502 0.8332 0.018 Uiso 1 1 calc R
H25B H 0.6255 0.9365 0.8756 0.018 Uiso 1 1 calc R
C26 C 0.6871(5) 1.0504(3) 0.7694(3) 0.0140(9) Uani 1 1 d .
H26A H 0.7683 1.1003 0.7518 0.017 Uiso 1 1 calc R
H26B H 0.6480 1.0922 0.8275 0.017 Uiso 1 1 calc R
C27 C 0.4048(6) 1.0680(3) 0.6644(3) 0.0214(10) Uani 1 1 d .
H27A H 0.3670 1.1032 0.7245 0.032 Uiso 1 1 calc R
H27B H 0.2949 1.0297 0.6092 0.032 Uiso 1 1 calc R
H27C H 0.4792 1.1211 0.6483 0.032 Uiso 1 1 calc R
N1 N 0.9892(5) 1.2186(3) 0.9703(3) 0.0223(9) Uani 1 1 d .
N2 N 1.0174(5) 1.2746(3) 0.9258(3) 0.0221(9) Uani 1 1 d .
N3 N 1.0381(8) 1.3323(4) 0.8860(4) 0.0494(14) Uani 1 1 d .
N4 N 1.2409(5) 1.0943(3) 0.8805(3) 0.0203(8) Uani 1 1 d .
N5 N 1.3460(5) 1.1771(3) 0.9034(2) 0.0126(7) Uani 1 1 d .
N6 N 1.4520(5) 1.2552(3) 0.9192(3) 0.0269(9) Uani 1 1 d .
N7 N 0.9073(5) 1.0583(3) 1.0452(3) 0.0160(8) Uani 1 1 d .
N8 N 0.7758(5) 1.0953(2) 1.0576(3) 0.0140(7) Uani 1 1 d .
N9 N 0.6497(6) 1.1305(3) 1.0684(4) 0.0351(11) Uani 1 1 d .
N11 N 0.7018(4) 0.4541(3) 0.1728(2) 0.0124(7) Uani 1 1 d .
N12 N 0.4242(5) 0.5265(3) 0.1574(3) 0.0186(8) Uani 1 1 d .
N13 N 0.4520(5) 0.4025(3) 0.2426(3) 0.0156(7) Uani 1 1 d .
N21 N 0.5161(4) 0.9919(3) 0.6818(2) 0.0125(7) Uani 1 1 d .
N22 N 0.5071(5) 0.8393(3) 0.7337(3) 0.0155(7) Uani 1 1 d .
N23 N 0.7897(4) 0.9788(2) 0.7958(2) 0.0116(7) Uani 1 1 d .
O10 O 0.2517(5) 0.6260(3) 0.4158(3) 0.0470(10) Uani 1 1 d .
P1 P 0.66355(15) 0.60571(8) 0.34446(8) 0.0135(2) Uani 1 1 d .
P2 P 0.71242(14) 0.84095(8) 0.60016(8) 0.0107(2) Uani 1 1 d .
Cu1 Cu 0.82475(7) 0.73989(4) 0.48375(4) 0.01468(12) Uani 1 1 d .
Cu2 Cu 1.04844(7) 1.08074(4) 0.94881(4) 0.01210(12) Uani 1 1 d .
I1 I 1.05099(4) 0.84338(2) 0.41451(2) 0.02500(9) Uani 1 1 d .
I2 I 0.98737(4) 0.65087(2) 0.60319(2) 0.02664(9) Uani 1 1 d .
H10A H 0.2012 0.6884 0.4179 0.032 Uiso 1 1 d .
H10B H 0.1685 0.5989 0.4361 0.032 Uiso 1 1 d .
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'
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'
I I -0.4742 1.8119 '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
N11 C11 P1 112.6(3) . .
N11 C11 H11A 109.1 . .
P1 C11 H11A 109.1 . .
N11 C11 H11B 109.1 . .
P1 C11 H11B 109.1 . .
H11A C11 H11B 107.8 . .
N12 C12 P1 111.7(3) . .
N12 C12 H12A 109.3 . .
P1 C12 H12A 109.3 . .
N12 C12 H12B 109.3 . .
P1 C12 H12B 109.3 . .
H12A C12 H12B 107.9 . .
N13 C13 P1 112.3(3) . .
N13 C13 H13A 109.1 . .
P1 C13 H13A 109.1 . .
N13 C13 H13B 109.1 . .
P1 C13 H13B 109.1 . .
H13A C13 H13B 107.9 . .
N12 C14 N11 112.5(3) . .
N12 C14 H14A 109.1 . .
N11 C14 H14A 109.1 . .
N12 C14 H14B 109.1 . .
N11 C14 H14B 109.1 . .
H14A C14 H14B 107.8 . .
N13 C15 N11 111.7(3) . .
N13 C15 H15A 109.3 . .
N11 C15 H15A 109.3 . .
N13 C15 H15B 109.3 . .
N11 C15 H15B 109.3 . .
H15A C15 H15B 108.0 . .
N12 C16 N13 113.1(3) . .
N12 C16 H16A 109.0 . .
N13 C16 H16A 109.0 . .
N12 C16 H16B 109.0 . .
N13 C16 H16B 109.0 . .
H16A C16 H16B 107.8 . .
N11 C17 H17A 109.5 . .
N11 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
N11 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
N21 C21 P2 113.4(3) . .
N21 C21 H21A 108.9 . .
P2 C21 H21A 108.9 . .
N21 C21 H21B 108.9 . .
P2 C21 H21B 108.9 . .
H21A C21 H21B 107.7 . .
N22 C22 P2 112.6(3) . .
N22 C22 H22A 109.1 . .
P2 C22 H22A 109.1 . .
N22 C22 H22B 109.1 . .
P2 C22 H22B 109.1 . .
H22A C22 H22B 107.8 . .
N23 C23 P2 112.5(3) . .
N23 C23 H23A 109.1 . .
P2 C23 H23A 109.1 . .
N23 C23 H23B 109.1 . .
P2 C23 H23B 109.1 . .
H23A C23 H23B 107.8 . .
N22 C24 N21 111.2(3) . .
N22 C24 H24A 109.4 . .
N21 C24 H24A 109.4 . .
N22 C24 H24B 109.4 . .
N21 C24 H24B 109.4 . .
H24A C24 H24B 108.0 . .
N22 C25 N23 112.9(3) . .
N22 C25 H25A 109.0 . .
N23 C25 H25A 109.0 . .
N22 C25 H25B 109.0 . .
N23 C25 H25B 109.0 . .
H25A C25 H25B 107.8 . .
N23 C26 N21 112.3(3) . .
N23 C26 H26A 109.1 . .
N21 C26 H26A 109.1 . .
N23 C26 H26B 109.1 . .
N21 C26 H26B 109.1 . .
H26A C26 H26B 107.9 . .
N21 C27 H27A 109.5 . .
N21 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
N21 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
N2 N1 Cu2 127.3(3) . .
N3 N2 N1 175.7(5) . .
N5 N4 Cu2 120.9(3) . .
N6 N5 N4 175.0(4) . .
N8 N7 Cu2 127.7(3) . 2_777
N8 N7 Cu2 122.5(3) . .
Cu2 N7 Cu2 103.06(14) 2_777 .
N9 N8 N7 179.4(5) . .
C17 N11 C11 109.6(3) . .
C17 N11 C14 109.7(3) . .
C11 N11 C14 110.2(3) . .
C17 N11 C15 108.5(3) . .
C11 N11 C15 111.1(3) . .
C14 N11 C15 107.7(3) . .
C14 N12 C16 110.2(3) . .
C14 N12 C12 112.3(3) . .
C16 N12 C12 112.0(3) . .
C15 N13 C16 110.0(3) . .
C15 N13 C13 111.9(3) . .
C16 N13 C13 112.4(3) . .
C27 N21 C21 109.1(3) . .
C27 N21 C26 110.1(3) . .
C21 N21 C26 110.4(3) . .
C27 N21 C24 109.7(3) . .
C21 N21 C24 109.7(3) . .
C26 N21 C24 107.9(3) . .
C24 N22 C25 110.6(3) . .
C24 N22 C22 113.4(3) . .
C25 N22 C22 111.8(3) . .
C26 N23 C25 110.0(3) . .
C26 N23 C23 112.0(3) . .
C25 N23 C23 111.4(3) . .
H10A O10 H10B 94.6 . .
C13 P1 C12 99.4(2) . .
C13 P1 C11 96.66(18) . .
C12 P1 C11 97.2(2) . .
C13 P1 Cu1 122.93(15) . .
C12 P1 Cu1 122.21(14) . .
C11 P1 Cu1 112.84(14) . .
C22 P2 C21 96.91(19) . .
C22 P2 C23 98.46(18) . .
C21 P2 C23 97.47(18) . .
C22 P2 Cu1 115.15(13) . .
C21 P2 Cu1 126.93(13) . .
C23 P2 Cu1 116.68(13) . .
P2 Cu1 P1 126.83(5) . .
P2 Cu1 I1 115.38(4) . .
P1 Cu1 I1 100.82(4) . .
P2 Cu1 I2 93.23(4) . .
P1 Cu1 I2 105.69(4) . .
I1 Cu1 I2 115.01(4) . .
N1 Cu2 N4 98.64(15) . .
N1 Cu2 N7 167.16(15) . 2_777
N4 Cu2 N7 92.52(14) . 2_777
N1 Cu2 N7 90.76(14) . .
N4 Cu2 N7 163.67(16) . .
N7 Cu2 N7 76.94(14) 2_777 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C11 N11 1.504(5) .
C11 P1 1.851(4) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 N12 1.475(5) .
C12 P1 1.846(5) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 N13 1.475(5) .
C13 P1 1.837(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 N12 1.432(6) .
C14 N11 1.525(5) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 N13 1.436(5) .
C15 N11 1.535(5) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 N12 1.465(6) .
C16 N13 1.464(6) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 N11 1.497(5) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C21 N21 1.519(5) .
C21 P2 1.841(4) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 N22 1.467(5) .
C22 P2 1.834(4) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 N23 1.484(5) .
C23 P2 1.842(4) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 N22 1.428(5) .
C24 N21 1.551(5) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 N22 1.459(5) .
C25 N23 1.479(5) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 N23 1.443(5) .
C26 N21 1.534(5) .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C27 N21 1.490(5) .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
N1 N2 1.191(5) .
N1 Cu2 1.948(4) .
N2 N3 1.146(6) .
N4 N5 1.193(5) .
N4 Cu2 1.955(3) .
N5 N6 1.168(5) .
N7 N8 1.202(5) .
N7 Cu2 2.014(3) 2_777
N7 Cu2 2.021(3) .
N8 N9 1.147(5) .
O10 H10A 0.982 .
O10 H10B 0.842 .
P1 Cu1 2.2314(12) .
P2 Cu1 2.2259(11) .
Cu1 I1 2.6438(9) .
Cu1 I2 2.6756(7) .
Cu2 N7 2.014(3) 2_777
