#------------------------------------------------------------------------------
#$Date: 2020-03-05 04:32:44 +0200 (Thu, 05 Mar 2020) $
#$Revision: 249065 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557475.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_1557475
loop_
_publ_author_name
'Arakawa, Kazuki'
'Yano, Natsumi'
'Imasaki, Nanako'
'Kohara, Yoshihiro'
'Yatsushiro, Daiki'
'Atarashi, Daiki'
'Handa, Makoto'
'Kataoka, Yusuke'
_publ_section_title
;
 Coordination-Induced Self-Assembly of a Heteroleptic Paddlewheel-Type
 Dirhodium Complex
;
_journal_issue                   2
_journal_name_full               Crystals
_journal_page_first              85
_journal_paper_doi               10.3390/cryst10020085
_journal_volume                  10
_journal_year                    2020
_chemical_formula_sum            'C16 H22 N2 O9 Rh2'
_chemical_formula_weight         592.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.077(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1042(11)
_cell_length_b                   14.3559(18)
_cell_length_c                   17.696(3)
_cell_measurement_reflns_used    7228
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.36
_cell_volume                     2005.4(5)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16890
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.580
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    1.697
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0653P)²+17.9008P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3123
_reflns_number_total             3505
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            CIF.cif
_cod_data_source_block           '[Rh2(O2CCH3)3(PABC)(DMF)]'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1557475
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.657
_shelx_estimated_absorpt_t_max   0.951
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.10987(7) 0.12827(4) 0.21018(3) 0.0254(2) Uani 1 1 d . . . . .
Rh2 Rh 0.23973(7) -0.00924(4) 0.27211(3) 0.0264(2) Uani 1 1 d . . . . .
O1 O 0.0608(6) 0.1683(3) 0.3135(3) 0.0264(11) Uani 1 1 d . . . . .
O2 O 0.1880(6) 0.0393(4) 0.3722(3) 0.0279(11) Uani 1 1 d . . . . .
O3 O 0.3397(6) 0.1911(4) 0.2403(3) 0.0311(12) Uani 1 1 d . . . . .
O4 O 0.4642(6) 0.0587(4) 0.2952(3) 0.0303(12) Uani 1 1 d . . . . .
O5 O 0.1661(6) 0.0815(4) 0.1105(3) 0.0294(12) Uani 1 1 d . . . . .
O6 O 0.2846(6) -0.0503(4) 0.1679(3) 0.0291(12) Uani 1 1 d . . . . .
O7 O -0.1149(7) 0.0575(4) 0.1813(3) 0.0330(12) Uani 1 1 d . . . . .
O8 O 0.0070(7) -0.0714(4) 0.2431(3) 0.0310(12) Uani 1 1 d . . . . .
O9 O 0.3712(7) -0.1367(4) 0.3394(3) 0.0311(12) Uani 1 1 d . . . . .
N1 N -0.0252(7) 0.2392(4) 0.6564(3) 0.0216(12) Uani 1 1 d . . . . .
H1A H -0.0008 0.1939 0.6915 0.026 Uiso 1 1 calc R U . . .
H1B H -0.1363 0.2492 0.6477 0.026 Uiso 1 1 calc R U . . .
N2 N 0.4733(9) -0.2002(5) 0.4583(4) 0.0344(15) Uani 1 1 d . . . . .
C1 C 0.1118(9) 0.1155(5) 0.3712(4) 0.0250(15) Uani 1 1 d . . . . .
C2 C 0.0762(9) 0.1472(5) 0.4470(4) 0.0254(15) Uani 1 1 d . . . . .
C3 C -0.0110(10) 0.2307(6) 0.4502(5) 0.0319(17) Uani 1 1 d . . . . .
H3 H -0.0468 0.2663 0.4056 0.038 Uiso 1 1 calc R U . . .
C4 C -0.0438(9) 0.2602(5) 0.5195(4) 0.0287(17) Uani 1 1 d . . . . .
H4 H -0.1019 0.3156 0.5216 0.034 Uiso 1 1 calc R U . . .
C5 C 0.0107(9) 0.2061(6) 0.5870(4) 0.0289(16) Uani 1 1 d . . . . .
C6 C 0.1008(10) 0.1260(6) 0.5838(5) 0.0327(18) Uani 1 1 d . . . . .
H6 H 0.1414 0.0916 0.6287 0.039 Uiso 1 1 calc R U . . .
C7 C 0.1316(10) 0.0962(6) 0.5139(5) 0.0317(17) Uani 1 1 d . . . . .
H7 H 0.1906 0.0410 0.5120 0.038 Uiso 1 1 calc R U . . .
C8 C 0.4646(10) 0.1417(6) 0.2733(5) 0.0329(18) Uani 1 1 d . . . . .
C9 C 0.6377(11) 0.1892(7) 0.2875(5) 0.045(2) Uani 1 1 d . . . . .
H9A H 0.6241 0.2521 0.2688 0.053 Uiso 1 1 calc R U . . .
H9B H 0.6882 0.1895 0.3421 0.053 Uiso 1 1 calc R U . . .
H9C H 0.7096 0.1558 0.2606 0.053 Uiso 1 1 calc R U . . .
C10 C 0.2399(9) 0.0046(5) 0.1112(4) 0.0247(16) Uani 1 1 d . . . . .
C11 C 0.2819(11) -0.0235(6) 0.0355(5) 0.0374(19) Uani 1 1 d . . . . .
H11A H 0.3379 -0.0829 0.0416 0.045 Uiso 1 1 calc R U . . .
H11B H 0.1794 -0.0279 -0.0041 0.045 Uiso 1 1 calc R U . . .
H11C H 0.3551 0.0223 0.0208 0.045 Uiso 1 1 calc R U . . .
C12 C -0.1187(10) -0.0250(6) 0.2046(5) 0.0312(17) Uani 1 1 d . . . . .
C13 C -0.2858(11) -0.0754(7) 0.1849(5) 0.045(2) Uani 1 1 d . . . . .
H13A H -0.2718 -0.1373 0.2058 0.054 Uiso 1 1 calc R U . . .
H13B H -0.3671 -0.0424 0.2067 0.054 Uiso 1 1 calc R U . . .
H13C H -0.3252 -0.0785 0.1295 0.054 Uiso 1 1 calc R U . . .
C14 C 0.3975(10) -0.1335(5) 0.4108(5) 0.0328(18) Uani 1 1 d . . . . .
H14 H 0.3617 -0.0807 0.4330 0.039 Uiso 1 1 calc R U . . .
C15 C 0.5395(12) -0.2801(6) 0.4277(5) 0.044(2) Uani 1 1 d . . . . .
H15A H 0.5897 -0.3212 0.4694 0.053 Uiso 1 1 calc R U . . .
H15B H 0.4496 -0.3120 0.3926 0.053 Uiso 1 1 calc R U . . .
H15C H 0.6239 -0.2611 0.4006 0.053 Uiso 1 1 calc R U . . .
C16 C 0.4835(12) -0.1959(7) 0.5406(5) 0.045(2) Uani 1 1 d . . . . .
H16A H 0.5424 -0.2498 0.5652 0.054 Uiso 1 1 calc R U . . .
H16B H 0.5437 -0.1407 0.5615 0.054 Uiso 1 1 calc R U . . .
H16C H 0.3713 -0.1944 0.5498 0.054 Uiso 1 1 calc R U . . .
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Rh1 O5 90.1(2) . . ?
O3 Rh1 O1 89.6(2) . . ?
O5 Rh1 O1 176.5(2) . . ?
O3 Rh1 O7 176.6(2) . . ?
O5 Rh1 O7 88.9(2) . . ?
O1 Rh1 O7 91.2(2) . . ?
O3 Rh1 N1 93.6(2) . 4_565 ?
O5 Rh1 N1 95.4(2) . 4_565 ?
O1 Rh1 N1 88.1(2) . 4_565 ?
O7 Rh1 N1 89.7(2) . 4_565 ?
O3 Rh1 Rh2 87.95(15) . . ?
O5 Rh1 Rh2 87.88(15) . . ?
O1 Rh1 Rh2 88.64(14) . . ?
O7 Rh1 Rh2 88.79(15) . . ?
N1 Rh1 Rh2 176.38(15) 4_565 . ?
O4 Rh2 O2 90.7(2) . . ?
O4 Rh2 O8 176.1(2) . . ?
O2 Rh2 O8 90.4(2) . . ?
O4 Rh2 O6 89.2(2) . . ?
O2 Rh2 O6 176.2(2) . . ?
O8 Rh2 O6 89.4(2) . . ?
O4 Rh2 O9 89.4(2) . . ?
O2 Rh2 O9 89.1(2) . . ?
O8 Rh2 O9 94.3(2) . . ?
O6 Rh2 O9 94.6(2) . . ?
O4 Rh2 Rh1 88.66(14) . . ?
O2 Rh2 Rh1 87.71(14) . . ?
O8 Rh2 Rh1 87.69(15) . . ?
O6 Rh2 Rh1 88.52(15) . . ?
O9 Rh2 Rh1 176.26(14) . . ?
C1 O1 Rh1 117.4(5) . . ?
C1 O2 Rh2 119.0(5) . . ?
C8 O3 Rh1 117.6(5) . . ?
C8 O4 Rh2 117.5(5) . . ?
C10 O5 Rh1 118.8(5) . . ?
C10 O6 Rh2 117.3(5) . . ?
C12 O7 Rh1 118.2(5) . . ?
C12 O8 Rh2 119.0(5) . . ?
C14 O9 Rh2 116.8(5) . . ?
C5 N1 Rh1 118.0(4) . 4_566 ?
C5 N1 H1A 107.8 . . ?
Rh1 N1 H1A 107.8 4_566 . ?
C5 N1 H1B 107.8 . . ?
Rh1 N1 H1B 107.8 4_566 . ?
H1A N1 H1B 107.1 . . ?
C14 N2 C15 120.0(7) . . ?
C14 N2 C16 121.4(7) . . ?
C15 N2 C16 118.5(7) . . ?
O2 C1 O1 127.2(7) . . ?
O2 C1 C2 116.4(6) . . ?
O1 C1 C2 116.4(6) . . ?
C7 C2 C3 119.3(7) . . ?
C7 C2 C1 120.9(7) . . ?
C3 C2 C1 119.7(7) . . ?
C4 C3 C2 120.0(7) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 119.9(7) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 N1 122.5(7) . . ?
C6 C5 C4 119.6(7) . . ?
N1 C5 C4 117.8(7) . . ?
C5 C6 C7 120.1(8) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C6 121.0(7) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
O4 C8 O3 128.1(8) . . ?
O4 C8 C9 116.1(7) . . ?
O3 C8 C9 115.8(7) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O5 C10 O6 127.4(7) . . ?
O5 C10 C11 115.4(7) . . ?
O6 C10 C11 117.1(7) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O7 C12 O8 126.2(7) . . ?
O7 C12 C13 117.6(7) . . ?
O8 C12 C13 116.1(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O9 C14 N2 124.7(8) . . ?
O9 C14 H14 117.7 . . ?
N2 C14 H14 117.7 . . ?
N2 C15 H15A 109.5 . . ?
N2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 O3 2.029(5) . ?
Rh1 O5 2.032(5) . ?
Rh1 O1 2.039(5) . ?
Rh1 O7 2.047(5) . ?
Rh1 N1 2.293(5) 4_565 ?
Rh1 Rh2 2.3840(8) . ?
Rh2 O4 2.023(5) . ?
Rh2 O2 2.033(5) . ?
Rh2 O8 2.044(5) . ?
Rh2 O6 2.046(5) . ?
Rh2 O9 2.308(5) . ?
O1 C1 1.263(9) . ?
O2 C1 1.254(9) . ?
O3 C8 1.266(10) . ?
O4 C8 1.253(10) . ?
O5 C10 1.255(9) . ?
O6 C10 1.262(9) . ?
O7 C12 1.256(10) . ?
O8 C12 1.277(10) . ?
O9 C14 1.234(10) . ?
N1 C5 1.406(9) . ?
N1 Rh1 2.292(5) 4_566 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C14 1.329(10) . ?
N2 C15 1.424(11) . ?
N2 C16 1.442(11) . ?
C1 C2 1.505(11) . ?
C2 C7 1.378(11) . ?
C2 C3 1.399(11) . ?
C3 C4 1.379(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.410(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.370(11) . ?
C6 C7 1.384(11) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.529(12) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.511(11) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.505(11) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
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
Rh2 O2 C1 O1 0.0(10) . . . . ?
Rh2 O2 C1 C2 179.6(5) . . . . ?
Rh1 O1 C1 O2 -1.3(10) . . . . ?
Rh1 O1 C1 C2 179.2(5) . . . . ?
O2 C1 C2 C7 2.6(10) . . . . ?
O1 C1 C2 C7 -177.7(7) . . . . ?
O2 C1 C2 C3 -178.9(7) . . . . ?
O1 C1 C2 C3 0.7(10) . . . . ?
C7 C2 C3 C4 -1.4(12) . . . . ?
C1 C2 C3 C4 -179.9(7) . . . . ?
C2 C3 C4 C5 0.1(11) . . . . ?
Rh1 N1 C5 C6 109.9(7) 4_566 . . . ?
Rh1 N1 C5 C4 -67.8(8) 4_566 . . . ?
C3 C4 C5 C6 2.1(11) . . . . ?
C3 C4 C5 N1 179.8(7) . . . . ?
N1 C5 C6 C7 179.6(7) . . . . ?
C4 C5 C6 C7 -2.8(12) . . . . ?
C3 C2 C7 C6 0.7(12) . . . . ?
C1 C2 C7 C6 179.2(7) . . . . ?
C5 C6 C7 C2 1.5(12) . . . . ?
Rh2 O4 C8 O3 2.7(11) . . . . ?
Rh2 O4 C8 C9 -176.6(6) . . . . ?
Rh1 O3 C8 O4 -5.3(11) . . . . ?
Rh1 O3 C8 C9 174.1(6) . . . . ?
Rh1 O5 C10 O6 0.7(10) . . . . ?
Rh1 O5 C10 C11 -178.1(5) . . . . ?
Rh2 O6 C10 O5 -2.1(10) . . . . ?
Rh2 O6 C10 C11 176.7(5) . . . . ?
Rh1 O7 C12 O8 -2.5(11) . . . . ?
Rh1 O7 C12 C13 178.4(6) . . . . ?
Rh2 O8 C12 O7 0.4(11) . . . . ?
Rh2 O8 C12 C13 179.6(6) . . . . ?
Rh2 O9 C14 N2 -179.2(6) . . . . ?
C15 N2 C14 O9 3.7(13) . . . . ?
C16 N2 C14 O9 -173.3(8) . . . . ?
