#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:29:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179450 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/47/4334774.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_4334774
loop_
_publ_author_name
'Kazuhiro Uemura'
'Masahiro Ebihara'
_publ_section_title
;
 Paramagnetic One-Dimensional Chains Comprised of Trinuclear Pt-Cu-Pt and
 Paddlewheel Dirhodium Complexes with Metal-Metal Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5535
_journal_page_last               5550
_journal_paper_doi               10.1021/ic400470g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C28 H64 Cu F12 N8 O12 P2 Pt2 Rh2'
_chemical_formula_weight         1654.35
_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                113.200(4)
_cell_angle_beta                 99.391(2)
_cell_angle_gamma                108.533(4)
_cell_formula_units_Z            1
_cell_length_a                   11.259(5)
_cell_length_b                   11.690(6)
_cell_length_c                   12.126(6)
_cell_measurement_reflns_used    4505
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.7573
_cell_measurement_theta_min      2.0901
_cell_volume                     1312.5(11)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        CRYSTALCLEAR
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0903
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10281
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    6.484
_exptl_absorpt_correction_T_max  0.4430
_exptl_absorpt_correction_T_min  0.2465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_description       block
_exptl_crystal_F_000             797
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         6.198
_refine_diff_density_min         -4.685
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0803P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                5023
_reflns_number_total             5903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400470g_si_002_3.cif
_cod_data_source_block           4
_cod_database_code               4334774
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
Pt1 Pt 0.26403(3) 0.29241(3) 0.33395(3) 0.02046(13) Uani 1 1 d .
Rh1 Rh 0.08615(6) 0.08923(6) 0.09521(6) 0.01833(17) Uani 1 1 d .
Cu1 Cu 0.5000 0.5000 0.5000 0.0202(3) Uani 1 2 d S
O4 O 0.1990(5) 0.1234(5) -0.0145(6) 0.0202(13) Uani 1 1 d .
O2 O 0.4850(6) 0.5953(6) 0.3998(6) 0.0274(15) Uani 1 1 d .
O1 O 0.5856(6) 0.4067(6) 0.3925(6) 0.0304(16) Uani 1 1 d .
N3 N 0.3903(8) 0.2158(7) 0.2808(7) 0.0274(19) Uani 1 1 d .
H10 H 0.3557 0.1261 0.2330 0.033 Uiso 1 1 calc R
N4 N 0.3008(8) 0.4092(7) 0.2482(7) 0.0253(18) Uani 1 1 d .
H20 H 0.2438 0.3748 0.1722 0.030 Uiso 1 1 calc R
N2 N 0.2263(9) 0.1696(8) 0.4219(8) 0.041(2) Uani 1 1 d .
H24 H 0.3044 0.1841 0.4728 0.061 Uiso 1 1 calc R
H25 H 0.1835 0.0797 0.3616 0.061 Uiso 1 1 calc R
H26 H 0.1745 0.1913 0.4697 0.061 Uiso 1 1 calc R
N1 N 0.1317(8) 0.3716(8) 0.3884(8) 0.034(2) Uani 1 1 d .
H21 H 0.0787 0.3200 0.4160 0.050 Uiso 1 1 calc R
H22 H 0.0809 0.3702 0.3209 0.050 Uiso 1 1 calc R
H23 H 0.1770 0.4596 0.4523 0.050 Uiso 1 1 calc R
C1 C 0.5216(9) 0.2811(8) 0.3071(9) 0.025(2) Uani 1 1 d .
C6 C 0.3983(8) 0.5300(8) 0.2900(8) 0.0212(18) Uani 1 1 d .
C2 C 0.5985(10) 0.2138(9) 0.2346(10) 0.035(2) Uani 1 1 d .
C3 C 0.5260(12) 0.0563(10) 0.1712(12) 0.045(3) Uani 1 1 d .
H1 H 0.5088 0.0287 0.2356 0.067 Uiso 1 1 calc R
H2 H 0.5814 0.0153 0.1311 0.067 Uiso 1 1 calc R
H3 H 0.4416 0.0247 0.1064 0.067 Uiso 1 1 calc R
P1 P 0.0020(3) 0.7073(4) 0.3523(3) 0.0484(8) Uani 1 1 d .
O6 O -0.0328(6) 0.0460(6) 0.1959(6) 0.0258(15) Uani 1 1 d .
C13 C 0.1489(9) 0.0529(8) -0.1355(9) 0.024(2) Uani 1 1 d .
C14 C 0.2263(9) 0.0924(9) -0.2122(10) 0.031(2) Uani 1 1 d .
H30 H 0.2052 0.1605 -0.2287 0.047 Uiso 1 1 calc R
H31 H 0.2036 0.0111 -0.2931 0.047 Uiso 1 1 calc R
H32 H 0.3213 0.1318 -0.1656 0.047 Uiso 1 1 calc R
F3 F 0.0470(10) 0.7892(10) 0.5016(9) 0.103(4) Uani 1 1 d .
C5 C 0.6138(14) 0.2610(11) 0.1362(13) 0.057(4) Uani 1 1 d .
H7 H 0.6732 0.3590 0.1788 0.086 Uiso 1 1 calc R
H8 H 0.5267 0.2458 0.0873 0.086 Uiso 1 1 calc R
H9 H 0.6513 0.2089 0.0787 0.086 Uiso 1 1 calc R
C4 C 0.7367(12) 0.2611(14) 0.3207(15) 0.085(7) Uani 1 1 d .
H4 H 0.7874 0.3592 0.3507 0.128 Uiso 1 1 calc R
H5 H 0.7813 0.2093 0.2734 0.128 Uiso 1 1 calc R
H6 H 0.7311 0.2455 0.3937 0.128 Uiso 1 1 calc R
F1 F -0.0489(16) 0.6133(14) 0.2087(10) 0.200(9) Uani 1 1 d .
F5 F -0.0161(16) 0.5839(12) 0.3824(15) 0.154(6) Uani 1 1 d .
F4 F -0.1412(10) 0.673(2) 0.3491(13) 0.189(8) Uani 1 1 d .
F6 F 0.0239(18) 0.8257(11) 0.3303(16) 0.194(8) Uani 1 1 d .
F2 F 0.1397(14) 0.728(3) 0.3580(19) 0.240(10) Uani 1 1 d .
O5 O 0.0140(6) 0.2223(6) 0.0785(6) 0.0243(14) Uani 1 1 d .
O3 O 0.1512(6) -0.0522(6) 0.1039(6) 0.0242(14) Uani 1 1 d .
C11 C 0.0854(8) -0.1765(8) 0.0185(9) 0.0213(18) Uani 1 1 d .
C7 C 0.4133(9) 0.5953(8) 0.2052(9) 0.026(2) Uani 1 1 d .
C8 C 0.2949(10) 0.5227(9) 0.0846(10) 0.035(2) Uani 1 1 d .
H11 H 0.2821 0.4276 0.0353 0.052 Uiso 1 1 calc R
H12 H 0.3109 0.5700 0.0338 0.052 Uiso 1 1 calc R
H13 H 0.2152 0.5235 0.1068 0.052 Uiso 1 1 calc R
C12 C 0.1276(9) -0.2820(9) 0.0348(10) 0.034(2) Uani 1 1 d .
H27 H 0.2234 -0.2391 0.0799 0.051 Uiso 1 1 calc R
H28 H 0.1069 -0.3585 -0.0490 0.051 Uiso 1 1 calc R
H29 H 0.0799 -0.3163 0.0839 0.051 Uiso 1 1 calc R
C9 C 0.5369(10) 0.5923(11) 0.1717(11) 0.040(3) Uani 1 1 d .
H14 H 0.6140 0.6443 0.2496 0.060 Uiso 1 1 calc R
H15 H 0.5508 0.6335 0.1158 0.060 Uiso 1 1 calc R
H16 H 0.5257 0.4970 0.1280 0.060 Uiso 1 1 calc R
C10 C 0.4350(12) 0.7426(10) 0.2760(11) 0.045(3) Uani 1 1 d .
H17 H 0.3563 0.7466 0.2987 0.067 Uiso 1 1 calc R
H18 H 0.4508 0.7859 0.2219 0.067 Uiso 1 1 calc R
H19 H 0.5123 0.7914 0.3535 0.067 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
Pt Pt -1.7033 8.3905 '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'
Rh Rh -1.1178 0.9187 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 '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
N3 Pt1 N4 92.9(3) . .
N3 Pt1 N1 179.7(3) . .
N4 Pt1 N1 87.0(3) . .
N3 Pt1 N2 86.6(4) . .
N4 Pt1 N2 179.5(3) . .
N1 Pt1 N2 93.4(4) . .
N3 Pt1 Cu1 78.1(2) . .
N4 Pt1 Cu1 78.6(2) . .
N1 Pt1 Cu1 102.2(2) . .
N2 Pt1 Cu1 101.6(2) . .
N3 Pt1 Rh1 84.9(2) . .
N4 Pt1 Rh1 84.2(2) . .
N1 Pt1 Rh1 94.8(2) . .
N2 Pt1 Rh1 95.5(2) . .
Cu1 Pt1 Rh1 155.010(19) . .
O5 Rh1 O6 91.2(3) . .
O5 Rh1 O3 177.1(2) . .
O6 Rh1 O3 88.7(3) . .
O5 Rh1 O4 89.4(3) . .
O6 Rh1 O4 177.0(2) . .
O3 Rh1 O4 90.6(3) . .
O5 Rh1 Rh1 88.83(17) . 2
O6 Rh1 Rh1 89.30(17) . 2
O3 Rh1 Rh1 88.30(17) . 2
O4 Rh1 Rh1 87.75(16) . 2
O5 Rh1 Pt1 90.32(17) . .
O6 Rh1 Pt1 83.36(17) . .
O3 Rh1 Pt1 92.52(17) . .
O4 Rh1 Pt1 99.60(16) . .
Rh1 Rh1 Pt1 172.59(5) 2 .
O1 Cu1 O1 179.997(1) 2_666 .
O1 Cu1 O2 89.9(3) 2_666 2_666
O1 Cu1 O2 90.1(3) . 2_666
O1 Cu1 O2 90.1(3) 2_666 .
O1 Cu1 O2 89.9(3) . .
O2 Cu1 O2 180.0(2) 2_666 .
O1 Cu1 Pt1 91.89(17) 2_666 .
O1 Cu1 Pt1 88.11(17) . .
O2 Cu1 Pt1 91.54(16) 2_666 .
O2 Cu1 Pt1 88.46(16) . .
O1 Cu1 Pt1 88.11(17) 2_666 2_666
O1 Cu1 Pt1 91.89(17) . 2_666
O2 Cu1 Pt1 88.46(16) 2_666 2_666
O2 Cu1 Pt1 91.54(16) . 2_666
Pt1 Cu1 Pt1 180.0 . 2_666
C13 O4 Rh1 119.6(5) . .
C6 O2 Cu1 119.4(5) . .
C1 O1 Cu1 120.7(6) . .
C1 N3 Pt1 129.2(6) . .
C1 N3 H10 115.4 . .
Pt1 N3 H10 115.4 . .
C6 N4 Pt1 128.9(7) . .
C6 N4 H20 115.6 . .
Pt1 N4 H20 115.6 . .
Pt1 N2 H24 109.5 . .
Pt1 N2 H25 109.5 . .
H24 N2 H25 109.5 . .
Pt1 N2 H26 109.5 . .
H24 N2 H26 109.5 . .
H25 N2 H26 109.5 . .
Pt1 N1 H21 109.5 . .
Pt1 N1 H22 109.5 . .
H21 N1 H22 109.5 . .
Pt1 N1 H23 109.5 . .
H21 N1 H23 109.5 . .
H22 N1 H23 109.5 . .
O1 C1 N3 120.4(9) . .
O1 C1 C2 117.1(8) . .
N3 C1 C2 122.5(8) . .
O2 C6 N4 123.0(8) . .
O2 C6 C7 116.9(7) . .
N4 C6 C7 120.1(8) . .
C1 C2 C5 107.0(9) . .
C1 C2 C4 111.2(9) . .
C5 C2 C4 107.0(11) . .
C1 C2 C3 111.1(8) . .
C5 C2 C3 110.9(9) . .
C4 C2 C3 109.5(10) . .
C2 C3 H1 109.5 . .
C2 C3 H2 109.5 . .
H1 C3 H2 109.5 . .
C2 C3 H3 109.5 . .
H1 C3 H3 109.5 . .
H2 C3 H3 109.5 . .
F6 P1 F2 88.7(11) . .
F6 P1 F4 97.5(11) . .
F2 P1 F4 173.8(12) . .
F6 P1 F1 89.5(9) . .
F2 P1 F1 91.2(10) . .
F4 P1 F1 89.0(8) . .
F6 P1 F3 96.6(8) . .
F2 P1 F3 90.7(9) . .
F4 P1 F3 88.5(7) . .
F1 P1 F3 173.7(7) . .
F6 P1 F5 177.3(9) . .
F2 P1 F5 90.0(10) . .
F4 P1 F5 83.8(9) . .
F1 P1 F5 92.9(8) . .
F3 P1 F5 81.0(7) . .
C13 O6 Rh1 118.6(6) 2 .
O4 C13 O6 124.6(8) . 2
O4 C13 C14 118.2(7) . .
O6 C13 C14 117.1(8) 2 .
C13 C14 H30 109.5 . .
C13 C14 H31 109.5 . .
H30 C14 H31 109.5 . .
C13 C14 H32 109.5 . .
H30 C14 H32 109.5 . .
H31 C14 H32 109.5 . .
C2 C5 H7 109.5 . .
C2 C5 H8 109.5 . .
H7 C5 H8 109.5 . .
C2 C5 H9 109.5 . .
H7 C5 H9 109.5 . .
H8 C5 H9 109.5 . .
C2 C4 H4 109.5 . .
C2 C4 H5 109.5 . .
H4 C4 H5 109.5 . .
C2 C4 H6 109.5 . .
H4 C4 H6 109.5 . .
H5 C4 H6 109.5 . .
C11 O5 Rh1 118.1(5) 2 .
C11 O3 Rh1 118.1(6) . .
O3 C11 O5 126.5(8) . 2
O3 C11 C12 117.0(8) . .
O5 C11 C12 116.5(7) 2 .
C10 C7 C6 110.1(9) . .
C10 C7 C8 108.5(8) . .
C6 C7 C8 113.5(7) . .
C10 C7 C9 108.4(8) . .
C6 C7 C9 106.3(8) . .
C8 C7 C9 109.8(9) . .
C7 C8 H11 109.5 . .
C7 C8 H12 109.5 . .
H11 C8 H12 109.5 . .
C7 C8 H13 109.5 . .
H11 C8 H13 109.5 . .
H12 C8 H13 109.5 . .
C11 C12 H27 109.5 . .
C11 C12 H28 109.5 . .
H27 C12 H28 109.5 . .
C11 C12 H29 109.5 . .
H27 C12 H29 109.5 . .
H28 C12 H29 109.5 . .
C7 C9 H14 109.5 . .
C7 C9 H15 109.5 . .
H14 C9 H15 109.5 . .
C7 C9 H16 109.5 . .
H14 C9 H16 109.5 . .
H15 C9 H16 109.5 . .
C7 C10 H17 109.5 . .
C7 C10 H18 109.5 . .
H17 C10 H18 109.5 . .
C7 C10 H19 109.5 . .
H17 C10 H19 109.5 . .
H18 C10 H19 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 N3 1.973(9) .
Pt1 N4 2.003(7) .
Pt1 N1 2.056(9) .
Pt1 N2 2.085(8) .
Pt1 Cu1 2.7034(9) .
Pt1 Rh1 2.7749(11) .
Rh1 O5 2.030(6) .
Rh1 O6 2.032(6) .
Rh1 O3 2.040(6) .
Rh1 O4 2.047(6) .
Rh1 Rh1 2.3701(14) 2
Cu1 O1 1.943(7) 2_666
Cu1 O1 1.943(7) .
Cu1 O2 1.966(6) 2_666
Cu1 O2 1.966(6) .
Cu1 Pt1 2.7034(9) 2_666
O4 C13 1.277(10) .
O2 C6 1.269(10) .
O1 C1 1.278(10) .
N3 C1 1.344(12) .
N3 H10 0.8800 .
N4 C6 1.314(10) .
N4 H20 0.8800 .
N2 H24 0.9100 .
N2 H25 0.9100 .
N2 H26 0.9100 .
N1 H21 0.9100 .
N1 H22 0.9100 .
N1 H23 0.9100 .
C1 C2 1.510(14) .
C6 C7 1.504(12) .
C2 C5 1.511(17) .
C2 C4 1.512(15) .
C2 C3 1.540(13) .
C3 H1 0.9800 .
C3 H2 0.9800 .
C3 H3 0.9800 .
P1 F6 1.465(12) .
P1 F2 1.477(13) .
P1 F4 1.523(11) .
P1 F1 1.529(11) .
P1 F3 1.573(10) .
P1 F5 1.583(12) .
O6 C13 1.281(9) 2
C13 O6 1.281(9) 2
C13 C14 1.478(12) .
C14 H30 0.9800 .
C14 H31 0.9800 .
C14 H32 0.9800 .
C5 H7 0.9800 .
C5 H8 0.9800 .
C5 H9 0.9800 .
C4 H4 0.9800 .
C4 H5 0.9800 .
C4 H6 0.9800 .
O5 C11 1.271(10) 2
O3 C11 1.269(10) .
C11 O5 1.271(10) 2
C11 C12 1.524(13) .
C7 C10 1.503(13) .
C7 C8 1.517(13) .
C7 C9 1.520(14) .
C8 H11 0.9800 .
C8 H12 0.9800 .
C8 H13 0.9800 .
C12 H27 0.9800 .
C12 H28 0.9800 .
C12 H29 0.9800 .
C9 H14 0.9800 .
C9 H15 0.9800 .
C9 H16 0.9800 .
C10 H17 0.9800 .
C10 H18 0.9800 .
C10 H19 0.9800 .
