#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/55/2105504.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_2105504
loop_
_publ_author_name
'Ebihara, Masahiro'
'Fuma, Yasuhiro'
_publ_section_title
;
 Two- and three-dimensional assembled structures constructed from
 amidate-bridged paddlewheel complexes with group 6 oxometallate ions
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              480
_journal_page_last               489
_journal_paper_doi               10.1107/S2052519213024068
_journal_volume                  69
_journal_year                    2013
_chemical_formula_moiety         'C24 H48 Mo N8 O12 Rh4, 2.44(O H2)'
_chemical_formula_sum            'C24 H52.88 Mo N8 O14.44 Rh4'
_chemical_formula_weight         1191.52
_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                112.460(2)
_cell_angle_beta                 99.574(2)
_cell_angle_gamma                108.472(3)
_cell_formula_units_Z            2
_cell_length_a                   12.952(4)
_cell_length_b                   13.849(5)
_cell_length_c                   14.679(5)
_cell_measurement_reflns_used    6964
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2180.4(13)
_computing_cell_refinement       CrystalClear
_computing_data_collection
'CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17845
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.838
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         9884
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0362
_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)+(0.0235P)²+3.5108P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                8783
_reflns_number_total             9884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ry5054.cif
_cod_data_source_block           VIII
_cod_original_sg_symbol_H-M      'P -1         '
_cod_database_code               2105504
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh Rh1 0.96536(2) 0.03178(3) 0.44022(2) 0.02026(7) Uani d . 1 1 . .
Rh Rh2 0.93213(2) 0.40664(2) 0.48075(2) 0.02081(7) Uani d . 1 1 . .
Rh Rh3 0.57970(2) 0.04872(3) 0.07975(2) 0.02054(7) Uani d . 1 1 . .
Rh Rh4 0.55655(2) -0.00010(2) 0.44237(2) 0.01812(7) Uani d . 1 1 . .
N N1 0.8188(3) -0.1028(3) 0.3925(3) 0.0260(7) Uani d . 1 1 . .
H H1 0.7611 -0.1126 0.3448 0.031 Uiso calc R 1 1 . .
O O1 0.8775(2) -0.1655(2) 0.5049(2) 0.0284(6) Uani d . 1 1 . .
N N2 0.9303(3) 0.1340(3) 0.5567(2) 0.0248(7) Uani d . 1 1 . .
H H2 0.8995 0.1776 0.5457 0.030 Uiso calc R 1 1 . .
O O2 0.9859(2) 0.0700(3) 0.6692(2) 0.0292(6) Uani d . 1 1 . .
N N3 0.8766(3) 0.3867(3) 0.3379(3) 0.0276(7) Uani d . 1 1 . .
H H3 0.8172 0.3235 0.2928 0.033 Uiso calc R 1 1 . .
O O3 1.0050(2) 0.5602(2) 0.3692(2) 0.0290(6) Uani d . 1 1 . .
N N4 1.0517(3) 0.3537(3) 0.4450(3) 0.0277(7) Uani d . 1 1 . .
H H4 1.0382 0.2826 0.4292 0.033 Uiso calc R 1 1 . .
O O4 1.1814(2) 0.5266(2) 0.4753(2) 0.0305(6) Uani d . 1 1 . .
N N5 0.5087(3) 0.1573(3) 0.1341(3) 0.0303(8) Uani d . 1 1 B .
H H5 0.5429 0.2133 0.1974 0.036 Uiso calc R 1 1 . .
O O5 0.3553(3) 0.0656(3) -0.0139(2) 0.0368(7) Uani d . 1 1 . .
N N6 0.4856(3) -0.0595(3) 0.1213(2) 0.0278(7) Uani d . 1 1 . .
H H6 0.5140 -0.0524 0.1827 0.033 Uiso calc R 1 1 . .
O O6 0.3326(2) -0.1535(3) -0.0264(2) 0.0324(7) Uani d . 1 1 . .
N N7 0.6541(3) -0.0370(3) 0.5314(3) 0.0240(7) Uani d . 1 1 C .
H H7 0.7145 -0.0437 0.5164 0.029 Uiso calc R 1 1 . .
O O7 0.5501(2) -0.0394(2) 0.6407(2) 0.0274(6) Uani d . 1 1 . .
N N8 0.6433(3) 0.1648(3) 0.5391(2) 0.0228(6) Uani d . 1 1 . .
H H8 0.6987 0.2040 0.5239 0.027 Uiso calc R 1 1 . .
O O8 0.5434(2) 0.1708(2) 0.6529(2) 0.0264(6) Uani d . 1 1 . .
Mo Mo1 0.76942(2) 0.11035(3) 0.33011(2) 0.01589(7) Uani d . 1 1 . .
O O9 0.8928(2) 0.0823(2) 0.3257(2) 0.0268(6) Uani d . 1 1 . .
O O10 0.8080(2) 0.2355(2) 0.4486(2) 0.0226(5) Uani d . 1 1 . .
O O11 0.7270(2) 0.1361(2) 0.2252(2) 0.0239(6) Uani d . 1 1 . .
O O12 0.6568(2) -0.0043(2) 0.3284(2) 0.0215(5) Uani d . 1 1 . .
O O13 0.5799(3) 0.2864(4) 0.3722(3) 0.0672(11) Uani d . 1 1 . .
O O14 0.8897(8) -0.0055(14) 0.1111(6) 0.221(11) Uani d P 0.74(2) 1 . .
O O15 1.0649(16) 0.153(2) 0.0531(18) 0.249(17) Uani d P 0.50(3) 1 . .
O O16 0.897(2) 0.149(3) 0.092(3) 0.13(2) Uani d P 0.196(17) 1 . .
C C1 0.8021(3) -0.1784(4) 0.4275(3) 0.0267(8) Uani d . 1 1 . .
C C2 0.6908(4) -0.2856(4) 0.3772(4) 0.0424(11) Uani d . 1 1 . .
H H9 0.6612 -0.2963 0.4315 0.051 Uiso calc R 1 1 . .
H H10 0.6335 -0.2765 0.3324 0.051 Uiso calc R 1 1 . .
C C3 0.7077(6) -0.3900(6) 0.3133(6) 0.084(2) Uani d . 1 1 . .
H H11 0.7675 -0.3969 0.3566 0.126 Uiso calc R 1 1 . .
H H12 0.7305 -0.3826 0.2557 0.126 Uiso calc R 1 1 . .
H H13 0.6362 -0.4580 0.2862 0.126 Uiso calc R 1 1 . .
C C4 0.9512(3) 0.1391(3) 0.6491(3) 0.0256(8) Uani d . 1 1 . .
C C5 0.9325(4) 0.2274(4) 0.7360(4) 0.0405(11) Uani d . 1 1 . .
H H14 0.8548 0.1923 0.7381 0.049 Uiso calc R 1 1 . .
H H15 0.9367 0.2911 0.7205 0.049 Uiso calc R 1 1 . .
C C6 1.0187(6) 0.2749(5) 0.8422(4) 0.0650(17) Uani d . 1 1 . .
H H16 1.0961 0.3085 0.8406 0.097 Uiso calc R 1 1 . .
H H17 1.0114 0.2133 0.8605 0.097 Uiso calc R 1 1 . .
H H18 1.0041 0.3334 0.8937 0.097 Uiso calc R 1 1 . .
C C7 0.9226(3) 0.4611(3) 0.3067(3) 0.0271(8) Uani d . 1 1 . .
C C8 0.8835(4) 0.4327(4) 0.1936(3) 0.0436(12) Uani d . 1 1 . .
H H19 0.8135 0.3608 0.1561 0.052 Uiso calc R 1 1 . .
H H20 0.8644 0.4937 0.1880 0.052 Uiso calc R 1 1 . .
C C9 0.9726(6) 0.4202(7) 0.1435(5) 0.092(3) Uani d . 1 1 . .
H H21 0.9844 0.3534 0.1404 0.138 Uiso calc R 1 1 . .
H H22 1.0444 0.4884 0.1840 0.138 Uiso calc R 1 1 . .
H H23 0.9471 0.4106 0.0734 0.138 Uiso calc R 1 1 . .
C C10 1.1490(3) 0.4171(4) 0.4432(3) 0.0299(9) Uani d . 1 1 A .
C C11 1.2278(4) 0.3663(4) 0.4005(5) 0.0478(12) Uani d DU 1 1 . .
H H24A 1.2090 0.2930 0.4025 0.057 Uiso calc PR 0.610(11) 1 A 1
H H25A 1.2106 0.3492 0.3270 0.057 Uiso calc PR 0.610(11) 1 A 1
H H24B 1.3041 0.4277 0.4215 0.057 Uiso calc PR 0.390(11) 1 A 2
H H25B 1.2365 0.3145 0.4287 0.057 Uiso calc PR 0.390(11) 1 A 2
C C12A 1.3546(7) 0.4375(7) 0.4541(8) 0.056(3) Uani d PDU 0.610(11) 1 A 1
H H26A 1.3742 0.5129 0.4580 0.084 Uiso calc PR 0.610(11) 1 A 1
H H27A 1.3963 0.4001 0.4151 0.084 Uiso calc PR 0.610(11) 1 A 1
H H28A 1.3755 0.4455 0.5241 0.084 Uiso calc PR 0.610(11) 1 A 1
C C12B 1.1805(17) 0.3039(18) 0.2887(12) 0.097(7) Uani d PDU 0.390(11) 1 A 2
H H26B 1.1669 0.3541 0.2615 0.145 Uiso calc PR 0.390(11) 1 A 2
H H27B 1.1083 0.2389 0.2683 0.145 Uiso calc PR 0.390(11) 1 A 2
H H28B 1.2342 0.2764 0.2609 0.145 Uiso calc PR 0.390(11) 1 A 2
C C13 0.4130(4) 0.1480(4) 0.0786(3) 0.0366(10) Uani d DU 1 1 . .
C C14A 0.3707(11) 0.2417(11) 0.1198(8) 0.063(3) Uani d PDU 0.84(2) 1 B 1
H H29A 0.2901 0.2063 0.1152 0.075 Uiso calc PR 0.84(2) 1 B 1
H H30A 0.4160 0.2936 0.1935 0.075 Uiso calc PR 0.84(2) 1 B 1
C C15A 0.3792(19) 0.3085(12) 0.0627(11) 0.144(7) Uani d PDU 0.84(2) 1 B 1
H H31A 0.3483 0.2568 -0.0117 0.216 Uiso calc PR 0.84(2) 1 B 1
H H32A 0.4594 0.3588 0.0811 0.216 Uiso calc PR 0.84(2) 1 B 1
H H33A 0.3356 0.3543 0.0808 0.216 Uiso calc PR 0.84(2) 1 B 1
C C14B 0.357(4) 0.225(4) 0.131(3) 0.040(8) Uani d PDU 0.16(2) 1 B 2
H H29B 0.3198 0.1948 0.1733 0.048 Uiso calc PR 0.16(2) 1 B 2
H H30B 0.4184 0.3014 0.1792 0.048 Uiso calc PR 0.16(2) 1 B 2
C C15B 0.272(7) 0.238(6) 0.064(5) 0.13(2) Uani d PDU 0.16(2) 1 B 2
H H31B 0.2289 0.2716 0.1036 0.189 Uiso calc PR 0.16(2) 1 B 2
H H32B 0.2204 0.1636 0.0061 0.189 Uiso calc PR 0.16(2) 1 B 2
H H33B 0.3115 0.2883 0.0373 0.189 Uiso calc PR 0.16(2) 1 B 2
C C16 0.3832(4) -0.1410(4) 0.0623(3) 0.0321(9) Uani d . 1 1 . .
C C17 0.3223(4) -0.2285(5) 0.0946(4) 0.0539(15) Uani d . 1 1 . .
H H34 0.3462 -0.1932 0.1709 0.065 Uiso calc R 1 1 . .
H H35 0.2390 -0.2526 0.0682 0.065 Uiso calc R 1 1 . .
C C18 0.3484(7) -0.3315(6) 0.0540(6) 0.084(2) Uani d . 1 1 . .
H H36 0.4291 -0.3097 0.0875 0.126 Uiso calc R 1 1 . .
H H37 0.3321 -0.3621 -0.0208 0.126 Uiso calc R 1 1 . .
H H38 0.3010 -0.3897 0.0689 0.126 Uiso calc R 1 1 . .
C C19 0.6352(3) -0.0519(3) 0.6104(3) 0.0265(8) Uani d DU 1 1 . .
C C20A 0.7079(5) -0.0899(8) 0.6683(7) 0.0379(15) Uani d PDU 0.943(10) 1 C 1
H H39A 0.6635 -0.1709 0.6487 0.045 Uiso calc PR 0.943(10) 1 C 1
H H40A 0.7759 -0.0846 0.6460 0.045 Uiso calc PR 0.943(10) 1 C 1
C C21A 0.7474(5) -0.0209(6) 0.7854(4) 0.0575(19) Uani d PDU 0.943(10) 1 C 1
H H41A 0.6808 -0.0270 0.8086 0.086 Uiso calc PR 0.943(10) 1 C 1
H H42A 0.7936 0.0591 0.8060 0.086 Uiso calc PR 0.943(10) 1 C 1
H H43A 0.7932 -0.0504 0.8171 0.086 Uiso calc PR 0.943(10) 1 C 1
C C20B 0.732(6) -0.067(16) 0.668(13) 0.040(13) Uani d PDU 0.057(10) 1 C 2
H H39B 0.7628 -0.1120 0.6201 0.048 Uiso calc PR 0.057(10) 1 C 2
H H40B 0.7947 0.0074 0.7194 0.048 Uiso calc PR 0.057(10) 1 C 2
C C21B 0.672(8) -0.131(9) 0.721(8) 0.045(14) Uani d PDU 0.057(10) 1 C 2
H H41B 0.6064 -0.2010 0.6682 0.068 Uiso calc PR 0.057(10) 1 C 2
H H42B 0.6451 -0.0831 0.7696 0.068 Uiso calc PR 0.057(10) 1 C 2
H H43B 0.7249 -0.1503 0.7575 0.068 Uiso calc PR 0.057(10) 1 C 2
C C22 0.6242(3) 0.2204(3) 0.6245(3) 0.0246(8) Uani d . 1 1 D .
C C23 0.6999(4) 0.3472(3) 0.6949(3) 0.0340(9) Uani d DU 1 1 . .
H H44A 0.7507 0.3563 0.7579 0.041 Uiso calc PR 0.91(3) 1 D 1
H H45A 0.7486 0.3767 0.6588 0.041 Uiso calc PR 0.91(3) 1 D 1
H H44B 0.7205 0.3626 0.7680 0.041 Uiso calc PR 0.09(3) 1 D 2
H H45B 0.7711 0.3694 0.6781 0.041 Uiso calc PR 0.09(3) 1 D 2
C C24A 0.6327(6) 0.4177(5) 0.7263(11) 0.051(3) Uani d PDU 0.91(3) 1 D 1
H H46A 0.5882 0.3925 0.7664 0.076 Uiso calc PR 0.91(3) 1 D 1
H H47A 0.5810 0.4080 0.6644 0.076 Uiso calc PR 0.91(3) 1 D 1
H H48A 0.6853 0.4981 0.7686 0.076 Uiso calc PR 0.91(3) 1 D 1
C C24B 0.635(7) 0.416(6) 0.679(9) 0.055(15) Uani d PDU 0.09(3) 1 D 2
H H46B 0.6895 0.4916 0.6950 0.083 Uiso calc PR 0.09(3) 1 D 2
H H47B 0.5891 0.4235 0.7252 0.083 Uiso calc PR 0.09(3) 1 D 2
H H48B 0.5850 0.3767 0.6073 0.083 Uiso calc PR 0.09(3) 1 D 2
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'
Mo Mo -1.6832 0.6857 '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'
Rh Rh -1.1178 0.9187 '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
_geom_angle_publ_flag
N1 Rh1 N2 . . 94.51(14) ?
N1 Rh1 O2 . 2_756 88.21(13) ?
N2 Rh1 O2 . 2_756 174.84(11) ?
N1 Rh1 O1 . 2_756 175.65(11) ?
N2 Rh1 O1 . 2_756 86.26(13) ?
O2 Rh1 O1 2_756 2_756 90.70(12) ?
N1 Rh1 O9 . . 91.66(11) ?
N2 Rh1 O9 . . 94.46(11) ?
O2 Rh1 O9 2_756 . 89.84(10) ?
O1 Rh1 O9 2_756 . 92.55(10) ?
N1 Rh1 Rh1 . 2_756 85.39(9) ?
N2 Rh1 Rh1 . 2_756 86.14(9) ?
O2 Rh1 Rh1 2_756 2_756 89.71(8) ?
O1 Rh1 Rh1 2_756 2_756 90.39(7) ?
O9 Rh1 Rh1 . 2_756 177.03(7) y
N4 Rh2 N3 . . 90.09(14) ?
N4 Rh2 O3 . 2_766 90.80(13) ?
N3 Rh2 O3 . 2_766 175.78(12) ?
N4 Rh2 O4 . 2_766 175.64(13) ?
N3 Rh2 O4 . 2_766 91.35(13) ?
O3 Rh2 O4 2_766 2_766 87.47(12) ?
N4 Rh2 O10 . . 94.50(12) ?
N3 Rh2 O10 . . 95.81(11) ?
O3 Rh2 O10 2_766 . 88.23(10) ?
O4 Rh2 O10 2_766 . 89.44(11) ?
N4 Rh2 Rh2 . 2_766 85.71(10) ?
N3 Rh2 Rh2 . 2_766 85.29(9) ?
O3 Rh2 Rh2 2_766 2_766 90.66(8) ?
O4 Rh2 Rh2 2_766 2_766 90.31(8) ?
O10 Rh2 Rh2 . 2_766 178.87(7) y
N6 Rh3 N5 . . 92.05(15) ?
N6 Rh3 O5 . 2_655 88.86(14) ?
N5 Rh3 O5 . 2_655 175.88(12) ?
N6 Rh3 O6 . 2_655 175.75(12) ?
N5 Rh3 O6 . 2_655 88.12(14) ?
O5 Rh3 O6 2_655 2_655 90.68(13) ?
N6 Rh3 O11 . . 93.74(11) ?
N5 Rh3 O11 . . 94.04(12) ?
O5 Rh3 O11 2_655 . 89.91(11) ?
O6 Rh3 O11 2_655 . 90.49(10) ?
N6 Rh3 Rh3 . 2_655 86.15(9) ?
N5 Rh3 Rh3 . 2_655 86.83(10) ?
O5 Rh3 Rh3 2_655 2_655 89.22(9) ?
O6 Rh3 Rh3 2_655 2_655 89.61(8) ?
O11 Rh3 Rh3 . 2_655 179.13(7) y
N8 Rh4 N7 . . 90.44(13) ?
N8 Rh4 O7 . 2_656 88.66(12) ?
N7 Rh4 O7 . 2_656 175.56(12) ?
N8 Rh4 O8 . 2_656 175.50(11) ?
N7 Rh4 O8 . 2_656 90.52(13) ?
O7 Rh4 O8 2_656 2_656 90.05(11) ?
N8 Rh4 O12 . . 96.02(11) ?
N7 Rh4 O12 . . 96.51(11) ?
O7 Rh4 O12 2_656 . 87.91(10) ?
O8 Rh4 O12 2_656 . 88.23(10) ?
N8 Rh4 Rh4 . 2_656 85.49(9) ?
N7 Rh4 Rh4 . 2_656 85.07(9) ?
O7 Rh4 Rh4 2_656 2_656 90.53(8) ?
O8 Rh4 Rh4 2_656 2_656 90.22(8) ?
O12 Rh4 Rh4 . 2_656 177.80(6) y
C1 N1 Rh1 . . 124.7(3) ?
C1 N1 H1 . . 117.6 ?
Rh1 N1 H1 . . 117.6 ?
C1 O1 Rh1 . 2_756 116.7(2) ?
C4 N2 Rh1 . . 123.4(3) ?
C4 N2 H2 . . 118.3 ?
Rh1 N2 H2 . . 118.3 ?
C4 O2 Rh1 . 2_756 117.6(2) ?
C7 N3 Rh2 . . 124.7(3) ?
C7 N3 H3 . . 117.7 ?
Rh2 N3 H3 . . 117.7 ?
C7 O3 Rh2 . 2_766 116.9(2) ?
C10 N4 Rh2 . . 124.9(3) ?
C10 N4 H4 . . 117.6 ?
Rh2 N4 H4 . . 117.6 ?
C10 O4 Rh2 . 2_766 117.0(2) ?
C13 N5 Rh3 . . 122.7(3) ?
C13 N5 H5 . . 118.7 ?
Rh3 N5 H5 . . 118.7 ?
C13 O5 Rh3 . 2_655 118.7(3) ?
C16 N6 Rh3 . . 124.0(3) ?
C16 N6 H6 . . 118.0 ?
Rh3 N6 H6 . . 118.0 ?
C16 O6 Rh3 . 2_655 118.1(3) ?
C19 N7 Rh4 . . 125.4(3) ?
C19 N7 H7 . . 117.3 ?
Rh4 N7 H7 . . 117.3 ?
C19 O7 Rh4 . 2_656 117.4(2) ?
C22 N8 Rh4 . . 125.1(3) ?
C22 N8 H8 . . 117.5 ?
Rh4 N8 H8 . . 117.5 ?
C22 O8 Rh4 . 2_656 116.9(2) ?
O9 Mo1 O10 . . 107.90(13) y
O11 Mo1 O9 . . 108.53(12) y
O9 Mo1 O12 . . 111.38(12) y
O11 Mo1 O10 . . 109.17(12) y
O12 Mo1 O10 . . 108.12(12) y
O11 Mo1 O12 . . 111.64(12) y
Mo1 O9 Rh1 . . 119.29(13) y
Mo1 O10 Rh2 . . 122.07(13) y
Mo1 O11 Rh3 . . 136.57(14) y
Mo1 O12 Rh4 . . 129.21(13) y
O1 C1 N1 . . 122.4(4) ?
O1 C1 C2 . . 117.2(4) ?
N1 C1 C2 . . 120.4(4) ?
C3 C2 C1 . . 111.4(4) ?
C3 C2 H9 . . 109.3 ?
C1 C2 H9 . . 109.3 ?
C3 C2 H10 . . 109.3 ?
C1 C2 H10 . . 109.3 ?
H9 C2 H10 . . 108.0 ?
C2 C3 H11 . . 109.5 ?
C2 C3 H12 . . 109.5 ?
H11 C3 H12 . . 109.5 ?
C2 C3 H13 . . 109.5 ?
H11 C3 H13 . . 109.5 ?
H12 C3 H13 . . 109.5 ?
O2 C4 N2 . . 122.4(4) ?
O2 C4 C5 . . 117.8(3) ?
N2 C4 C5 . . 119.8(3) ?
C4 C5 C6 . . 113.7(4) ?
C4 C5 H14 . . 108.8 ?
C6 C5 H14 . . 108.8 ?
C4 C5 H15 . . 108.8 ?
C6 C5 H15 . . 108.8 ?
H14 C5 H15 . . 107.7 ?
C5 C6 H16 . . 109.5 ?
C5 C6 H17 . . 109.5 ?
H16 C6 H17 . . 109.5 ?
C5 C6 H18 . . 109.5 ?
H16 C6 H18 . . 109.5 ?
H17 C6 H18 . . 109.5 ?
O3 C7 N3 . . 122.3(4) ?
O3 C7 C8 . . 116.8(3) ?
N3 C7 C8 . . 120.9(4) ?
C9 C8 C7 . . 112.5(4) ?
C9 C8 H19 . . 109.1 ?
C7 C8 H19 . . 109.1 ?
C9 C8 H20 . . 109.1 ?
C7 C8 H20 . . 109.1 ?
H19 C8 H20 . . 107.8 ?
C8 C9 H21 . . 109.5 ?
C8 C9 H22 . . 109.5 ?
H21 C9 H22 . . 109.5 ?
C8 C9 H23 . . 109.5 ?
H21 C9 H23 . . 109.5 ?
H22 C9 H23 . . 109.5 ?
O4 C10 N4 . . 121.8(4) ?
O4 C10 C11 . . 116.7(4) ?
N4 C10 C11 . . 121.5(4) ?
C12B C11 C10 . . 109.5(8) ?
C12A C11 C10 . . 117.0(5) ?
C12A C11 H24A . . 108.0 ?
C10 C11 H24A . . 108.0 ?
C12A C11 H25A . . 108.0 ?
C10 C11 H25A . . 108.0 ?
H24A C11 H25A . . 107.3 ?
C12B C11 H24B . . 109.8 ?
C10 C11 H24B . . 109.8 ?
C12B C11 H25B . . 109.8 ?
C10 C11 H25B . . 109.8 ?
H24B C11 H25B . . 108.2 ?
C11 C12A H26A . . 109.5 ?
C11 C12A H27A . . 109.5 ?
H26A C12A H27A . . 109.5 ?
C11 C12A H28A . . 109.5 ?
H26A C12A H28A . . 109.5 ?
H27A C12A H28A . . 109.5 ?
C11 C12B H26B . . 109.5 ?
C11 C12B H27B . . 109.5 ?
H26B C12B H27B . . 109.5 ?
C11 C12B H28B . . 109.5 ?
H26B C12B H28B . . 109.5 ?
H27B C12B H28B . . 109.5 ?
O5 C13 N5 . . 122.5(4) ?
O5 C13 C14B . . 118(2) ?
N5 C13 C14B . . 118.8(19) ?
O5 C13 C14A . . 117.3(5) ?
N5 C13 C14A . . 120.0(6) ?
C15A C14A C13 . . 112.9(7) ?
C15A C14A H29A . . 109.0 ?
C13 C14A H29A . . 109.0 ?
C15A C14A H30A . . 109.0 ?
C13 C14A H30A . . 109.0 ?
H29A C14A H30A . . 107.8 ?
C14A C15A H31A . . 109.5 ?
C14A C15A H32A . . 109.5 ?
H31A C15A H32A . . 109.5 ?
C14A C15A H33A . . 109.5 ?
H31A C15A H33A . . 109.5 ?
H32A C15A H33A . . 109.5 ?
C15B C14B C13 . . 117(3) ?
C15B C14B H29B . . 108.0 ?
C13 C14B H29B . . 108.0 ?
C15B C14B H30B . . 108.0 ?
C13 C14B H30B . . 108.0 ?
H29B C14B H30B . . 107.2 ?
C14B C15B H31B . . 109.5 ?
C14B C15B H32B . . 109.5 ?
H31B C15B H32B . . 109.5 ?
C14B C15B H33B . . 109.5 ?
H31B C15B H33B . . 109.5 ?
H32B C15B H33B . . 109.5 ?
O6 C16 N6 . . 122.0(4) ?
O6 C16 C17 . . 117.1(4) ?
N6 C16 C17 . . 120.8(3) ?
C18 C17 C16 . . 111.7(5) ?
C18 C17 H34 . . 109.3 ?
C16 C17 H34 . . 109.3 ?
C18 C17 H35 . . 109.3 ?
C16 C17 H35 . . 109.3 ?
H34 C17 H35 . . 108.0 ?
C17 C18 H36 . . 109.5 ?
C17 C18 H37 . . 109.5 ?
H36 C18 H37 . . 109.5 ?
C17 C18 H38 . . 109.5 ?
H36 C18 H38 . . 109.5 ?
H37 C18 H38 . . 109.5 ?
O7 C19 N7 . . 121.6(3) ?
O7 C19 C20A . . 116.4(4) ?
N7 C19 C20A . . 122.0(4) ?
O7 C19 C20B . . 126(5) ?
N7 C19 C20B . . 112(4) ?
C21A C20A C19 . . 114.2(6) ?
C21A C20A H39A . . 108.7 ?
C19 C20A H39A . . 108.7 ?
C21A C20A H40A . . 108.7 ?
C19 C20A H40A . . 108.7 ?
H39A C20A H40A . . 107.6 ?
C20A C21A H41A . . 109.5 ?
C20A C21A H42A . . 109.5 ?
H41A C21A H42A . . 109.5 ?
C20A C21A H43A . . 109.5 ?
H41A C21A H43A . . 109.5 ?
H42A C21A H43A . . 109.5 ?
C21B C20B C19 . . 102(4) ?
C21B C20B H39B . . 111.5 ?
C19 C20B H39B . . 111.5 ?
C21B C20B H40B . . 111.5 ?
C19 C20B H40B . . 111.5 ?
H39B C20B H40B . . 109.3 ?
C20B C21B H41B . . 109.5 ?
C20B C21B H42B . . 109.5 ?
H41B C21B H42B . . 109.5 ?
C20B C21B H43B . . 109.5 ?
H41B C21B H43B . . 109.5 ?
H42B C21B H43B . . 109.5 ?
O8 C22 N8 . . 122.3(4) ?
O8 C22 C23 . . 117.6(3) ?
N8 C22 C23 . . 120.1(3) ?
C24A C23 C22 . . 113.2(4) ?
C24B C23 C22 . . 109(3) ?
C24A C23 H44A . . 108.9 ?
C22 C23 H44A . . 108.9 ?
C24A C23 H45A . . 108.9 ?
C22 C23 H45A . . 108.9 ?
H44A C23 H45A . . 107.7 ?
C24B C23 H44B . . 109.9 ?
C22 C23 H44B . . 109.9 ?
C24A C23 H45B . . 127.0 ?
C24B C23 H45B . . 109.9 ?
C22 C23 H45B . . 109.9 ?
H44B C23 H45B . . 108.3 ?
C23 C24A H46A . . 109.5 ?
C23 C24A H47A . . 109.5 ?
H46A C24A H47A . . 109.5 ?
C23 C24A H48A . . 109.5 ?
H46A C24A H48A . . 109.5 ?
H47A C24A H48A . . 109.5 ?
C23 C24B H46B . . 109.5 ?
C23 C24B H47B . . 109.5 ?
H46B C24B H47B . . 109.5 ?
C23 C24B H48B . . 109.5 ?
H46B C24B H48B . . 109.5 ?
H47B C24B H48B . . 109.5 ?
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
Rh1 N1 . 1.971(3) y
Rh1 N2 . 1.987(3) y
Rh1 O1 2_756 2.036(3) y
Rh1 O2 2_756 2.034(3) y
Rh1 O9 . 2.233(2) y
Rh1 Rh1 2_756 2.4117(8) y
Rh2 N3 . 1.980(3) y
Rh2 N4 . 1.977(3) y
Rh2 O3 2_766 2.030(3) y
Rh2 O4 2_766 2.039(3) y
Rh2 O10 . 2.214(3) y
Rh2 Rh2 2_766 2.4019(9) y
Rh3 N5 . 1.986(3) y
Rh3 N6 . 1.972(3) y
Rh3 O5 2_655 2.025(3) y
Rh3 O6 2_655 2.032(3) y
Rh3 O11 . 2.207(2) y
Rh3 Rh3 2_655 2.4037(8) y
Rh4 N7 . 1.983(3) y
Rh4 N8 . 1.965(3) y
Rh4 O7 2_656 2.031(3) y
Rh4 O8 2_656 2.038(3) y
Rh4 O12 . 2.277(3) y
Rh4 Rh4 2_656 2.4148(8) y
N1 C1 . 1.309(5) ?
N1 H1 . 0.8700 ?
O1 C1 . 1.281(4) ?
N2 C4 . 1.308(5) ?
N2 H2 . 0.8700 ?
O2 C4 . 1.284(4) ?
N3 C7 . 1.301(5) ?
N3 H3 . 0.8700 ?
O3 C7 . 1.284(5) ?
N4 C10 . 1.298(5) ?
N4 H4 . 0.8700 ?
O4 C10 . 1.296(5) ?
N5 C13 . 1.304(5) ?
N5 H5 . 0.8700 ?
O5 C13 . 1.282(5) ?
N6 C16 . 1.306(5) ?
N6 H6 . 0.8700 ?
O6 C16 . 1.276(4) ?
N7 C19 . 1.301(5) ?
N7 H7 . 0.8700 ?
O7 C19 . 1.292(4) ?
N8 C22 . 1.308(5) ?
N8 H8 . 0.8700 ?
O8 C22 . 1.284(5) ?
Mo1 O11 . 1.750(2) ?
Mo1 O9 . 1.766(2) ?
Mo1 O12 . 1.771(3) ?
Mo1 O10 . 1.772(3) ?
C1 C2 . 1.510(6) ?
C2 C3 . 1.500(8) ?
C2 H9 . 0.9800 ?
C2 H10 . 0.9800 ?
C3 H11 . 0.9700 ?
C3 H12 . 0.9700 ?
C3 H13 . 0.9700 ?
C4 C5 . 1.510(6) ?
C5 C6 . 1.510(7) ?
C5 H14 . 0.9800 ?
C5 H15 . 0.9800 ?
C6 H16 . 0.9700 ?
C6 H17 . 0.9700 ?
C6 H18 . 0.9700 ?
C7 C8 . 1.504(6) ?
C8 C9 . 1.488(8) ?
C8 H19 . 0.9800 ?
C8 H20 . 0.9800 ?
C9 H21 . 0.9700 ?
C9 H22 . 0.9700 ?
C9 H23 . 0.9700 ?
C10 C11 . 1.504(6) ?
C11 C12B . 1.435(14) ?
C11 C12A . 1.497(9) ?
C11 H24A . 0.9800 ?
C11 H25A . 0.9800 ?
C11 H24B . 0.9800 ?
C11 H25B . 0.9800 ?
C12A H26A . 0.9700 ?
C12A H27A . 0.9700 ?
C12A H28A . 0.9700 ?
C12B H26B . 0.9700 ?
C12B H27B . 0.9700 ?
C12B H28B . 0.9700 ?
C13 C14B . 1.516(18) ?
C13 C14A . 1.520(7) ?
C14A C15A . 1.459(13) ?
C14A H29A . 0.9800 ?
C14A H30A . 0.9800 ?
C15A H31A . 0.9700 ?
C15A H32A . 0.9700 ?
C15A H33A . 0.9700 ?
C14B C15B . 1.46(2) ?
C14B H29B . 0.9800 ?
C14B H30B . 0.9800 ?
C15B H31B . 0.9700 ?
C15B H32B . 0.9700 ?
C15B H33B . 0.9700 ?
C16 C17 . 1.508(6) ?
C17 C18 . 1.492(9) ?
C17 H34 . 0.9800 ?
C17 H35 . 0.9800 ?
C18 H36 . 0.9700 ?
C18 H37 . 0.9700 ?
C18 H38 . 0.9700 ?
C19 C20A . 1.508(6) ?
C19 C20B . 1.51(2) ?
C20A C21A . 1.508(10) ?
C20A H39A . 0.9800 ?
C20A H40A . 0.9800 ?
C21A H41A . 0.9700 ?
C21A H42A . 0.9700 ?
C21A H43A . 0.9700 ?
C20B C21B . 1.51(2) ?
C20B H39B . 0.9800 ?
C20B H40B . 0.9800 ?
C21B H41B . 0.9700 ?
C21B H42B . 0.9700 ?
C21B H43B . 0.9700 ?
C22 C23 . 1.517(6) ?
C23 C24A . 1.501(7) ?
C23 C24B . 1.51(2) ?
C23 H44A . 0.9800 ?
C23 H45A . 0.9800 ?
C23 H44B . 0.9800 ?
C23 H45B . 0.9800 ?
C24A H46A . 0.9700 ?
C24A H47A . 0.9700 ?
C24A H48A . 0.9700 ?
C24B H46B . 0.9700 ?
C24B H47B . 0.9700 ?
C24B H48B . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 O12 . 0.87 2.36 3.049(4) 135.8
N2 H2 O10 . 0.87 2.24 3.048(4) 155.5
N3 H3 O11 . 0.87 2.19 2.970(4) 148.4
N4 H4 O9 . 0.87 2.46 3.210(4) 144.2
N4 H4 O1 2_756 0.87 2.59 3.307(4) 139.8
N5 H5 O13 . 0.87 2.27 3.061(5) 152.0
N6 H6 O12 . 0.87 2.29 3.107(4) 156.0
N7 H7 N1 . 0.87 2.49 3.286(5) 153.1
N8 H8 O10 . 0.87 1.98 2.808(4) 158.9
