#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/98/2239804.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_2239804
loop_
_publ_author_name
'Eagle, Cassandra T.'
'Quarshie, Fredricka'
'Cook, Kevin M.'
_publ_section_title
;
 (3-Methylbenzonitrile-1κN)-cis-tetrakis(μ-N-phenylacetamidato)-1:2κ⁴N:O;1:2κ⁴O:N-dirhodium(II)(Rh---Rh)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m304
_journal_paper_doi               10.1107/S1600536814016031
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Rh2 (C8 H8 N O)4 (C8 H7 N1)]'
_chemical_formula_moiety         'C40 H39 N5 O4 Rh2'
_chemical_formula_sum            'C40 H39 N5 O4 Rh2'
_chemical_formula_weight         859.59
_chemical_name_systematic
(3-Methylbenzonitrile-1κN)-cis-tetrakis(μ-N-phenylacetamidato)-1:2κ⁴N:O;1:2κ⁴O:N-dirhodium(II)(Rh---Rh)
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.3319(14)
_cell_length_b                   18.3248(16)
_cell_length_c                   12.9564(12)
_cell_measurement_reflns_used    27167
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      3.03
_cell_volume                     3640.2(6)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 2010)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 2010)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 2010)'
_computing_molecular_graphics    'CrystalStructure (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36328
_diffrn_reflns_theta_full        27.400
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         3.030
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Rigaku, 1998)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             1744.00
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.503
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0277P)²+7.3733P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                3154
_reflns_number_total             4292
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            mw2125sup1.cf
_cod_data_source_block           I
_cod_database_code               2239804
_cod_database_fobs_code          2239804
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           .2013
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2+Z
3 +X,1/2-Y,+Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 1/2+X,1/2-Y,1/2-Z
7 -X,1/2+Y,-Z
8 1/2+X,+Y,1/2-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_occupancy
Rh Rh1 0.47995(2) 0.2500 0.52236(3) 0.02157(11) Uani d 1
Rh Rh2 0.32933(2) 0.2500 0.46954(3) 0.02139(11) Uani d 1
O O1 0.35639(16) 0.32962(14) 0.36333(19) 0.0294(6) Uani d 1
O O2 0.44972(15) 0.16995(14) 0.62786(18) 0.0254(6) Uani d 1
N N1 0.49816(19) 0.33240(17) 0.4172(2) 0.0262(7) Uani d 1
N N2 0.30842(19) 0.17003(16) 0.5753(2) 0.0237(6) Uani d 1
N N3 0.6160(3) 0.2500 0.5704(4) 0.0336(11) Uani d 1
C C1 0.4333(2) 0.3578(2) 0.3624(3) 0.0273(8) Uani d 1
C C2 0.4427(3) 0.4243(2) 0.2942(3) 0.0401(10) Uani d 1
H H2A 0.4958 0.4501 0.3121 0.048 Uiso calc 1
H H2B 0.3930 0.4562 0.3043 0.048 Uiso calc 1
H H2C 0.4453 0.4092 0.2226 0.048 Uiso calc 1
C C3 0.3715(2) 0.1440(2) 0.6319(3) 0.0252(8) Uani d 1
C C4 0.3608(3) 0.0811(2) 0.7052(3) 0.0342(9) Uani d 1
H H4A 0.4090 0.0473 0.6966 0.041 Uiso calc 1
H H4B 0.3064 0.0562 0.6908 0.041 Uiso calc 1
H H4C 0.3602 0.0991 0.7756 0.041 Uiso calc 1
C C5 0.5811(2) 0.3681(2) 0.4141(3) 0.0283(8) Uani d 1
C C6 0.6393(3) 0.3544(2) 0.3362(3) 0.0342(9) Uani d 1
H H6 0.6232 0.3231 0.2819 0.041 Uiso calc 1
C C7 0.7218(3) 0.3860(2) 0.3363(3) 0.0386(10) Uani d 1
H H7 0.7611 0.3766 0.2822 0.046 Uiso calc 1
C C8 0.7452(3) 0.4311(2) 0.4159(4) 0.0428(11) Uani d 1
H H8 0.8008 0.4527 0.4163 0.051 Uiso calc 1
C C9 0.6879(3) 0.4451(3) 0.4957(4) 0.0457(11) Uani d 1
H H9 0.7047 0.4755 0.5506 0.055 Uiso calc 1
C C10 0.6056(3) 0.4140(2) 0.4942(3) 0.0373(10) Uani d 1
H H10 0.5661 0.4240 0.5478 0.045 Uiso calc 1
C C11 0.2218(2) 0.1406(2) 0.5787(3) 0.0270(8) Uani d 1
C C12 0.1718(3) 0.1409(2) 0.6679(3) 0.0344(9) Uani d 1
H H12 0.1944 0.1608 0.7291 0.041 Uiso calc 1
C C13 0.0885(3) 0.1117(2) 0.6669(4) 0.0423(11) Uani d 1
H H13 0.0555 0.1112 0.7280 0.051 Uiso calc 1
C C14 0.0535(3) 0.0835(2) 0.5780(4) 0.0464(12) Uani d 1
H H14 -0.0028 0.0633 0.5784 0.056 Uiso calc 1
C C15 0.1015(3) 0.0850(2) 0.4881(4) 0.0424(11) Uani d 1
H H15 0.0773 0.0668 0.4266 0.051 Uiso calc 1
C C16 0.1855(3) 0.1134(2) 0.4879(3) 0.0334(9) Uani d 1
H H16 0.2180 0.1142 0.4263 0.040 Uiso calc 1
C C17 0.6913(4) 0.2500 0.5696(5) 0.0339(13) Uani d 1
C C18 0.7854(3) 0.2500 0.5655(5) 0.0295(12) Uani d 1
C C19 0.8285(4) 0.2500 0.4693(4) 0.0331(13) Uani d 1
H H19 0.7953 0.2500 0.4083 0.040 Uiso calc 1
C C20 0.9168(4) 0.2500 0.4626(4) 0.0356(14) Uani d 1
C C21 0.9642(4) 0.2500 0.5533(4) 0.0315(13) Uani d 1
H H21 1.0255 0.2500 0.5501 0.038 Uiso calc 1
C C22 0.9239(4) 0.2500 0.6481(4) 0.0354(14) Uani d 1
H H22 0.9578 0.2500 0.7085 0.042 Uiso calc 1
C C23 0.8346(4) 0.2500 0.6552(4) 0.0317(13) Uani d 1
H H23 0.8072 0.2500 0.7200 0.038 Uiso calc 1
C C24 0.9623(5) 0.2500 0.3590(5) 0.0500(18) Uani d 1
H H24A 0.9234 0.2697 0.3070 0.060 Uiso calc 0.5
H H24B 0.9783 0.2004 0.3407 0.060 Uiso calc 0.5
H H24C 1.0144 0.2799 0.3630 0.060 Uiso calc 0.5
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rh Rh -1.1178 0.9187
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.0033 0.0016
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 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
N1 Rh1 N1 . 3 94.72(17)
N1 Rh1 O2 . 3 86.96(11)
N1 Rh1 O2 3 3 174.72(11)
N1 Rh1 O2 . . 174.72(11)
N1 Rh1 O2 3 . 86.96(11)
O2 Rh1 O2 3 . 90.92(14)
N1 Rh1 N3 . . 93.41(12)
N1 Rh1 N3 3 . 93.41(12)
O2 Rh1 N3 3 . 91.48(11)
O2 Rh1 N3 . . 91.48(11)
N1 Rh1 Rh2 . . 86.66(8)
N1 Rh1 Rh2 3 . 86.66(8)
O2 Rh1 Rh2 3 . 88.44(7)
O2 Rh1 Rh2 . . 88.44(7)
N3 Rh1 Rh2 . . 179.89(13)
N2 Rh2 N2 3 . 92.30(17)
N2 Rh2 O1 3 . 88.36(11)
N2 Rh2 O1 . . 177.38(11)
N2 Rh2 O1 3 3 177.38(11)
N2 Rh2 O1 . 3 88.36(11)
O1 Rh2 O1 . 3 90.86(15)
N2 Rh2 Rh1 3 . 87.68(8)
N2 Rh2 Rh1 . . 87.68(8)
O1 Rh2 Rh1 . . 89.81(7)
O1 Rh2 Rh1 3 . 89.81(7)
C1 O1 Rh2 . . 118.6(2)
C3 O2 Rh1 . . 119.9(2)
C1 N1 C5 . . 119.8(3)
C1 N1 Rh1 . . 121.3(2)
C5 N1 Rh1 . . 118.4(2)
C3 N2 C11 . . 122.2(3)
C3 N2 Rh2 . . 121.7(2)
C11 N2 Rh2 . . 116.0(2)
C17 N3 Rh1 . . 162.8(5)
O1 C1 N1 . . 123.2(3)
O1 C1 C2 . . 114.6(3)
N1 C1 C2 . . 122.2(3)
C1 C2 H2A . . 109.5
C1 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
C1 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
O2 C3 N2 . . 122.1(3)
O2 C3 C4 . . 114.2(3)
N2 C3 C4 . . 123.7(3)
C3 C4 H4A . . 109.5
C3 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C3 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
C6 C5 C10 . . 119.1(4)
C6 C5 N1 . . 121.0(4)
C10 C5 N1 . . 119.8(3)
C5 C6 C7 . . 121.0(4)
C5 C6 H6 . . 119.5
C7 C6 H6 . . 119.5
C8 C7 C6 . . 119.3(4)
C8 C7 H7 . . 120.3
C6 C7 H7 . . 120.3
C7 C8 C9 . . 120.7(4)
C7 C8 H8 . . 119.7
C9 C8 H8 . . 119.7
C8 C9 C10 . . 119.5(4)
C8 C9 H9 . . 120.2
C10 C9 H9 . . 120.2
C9 C10 C5 . . 120.4(4)
C9 C10 H10 . . 119.8
C5 C10 H10 . . 119.8
C12 C11 C16 . . 118.9(3)
C12 C11 N2 . . 122.5(3)
C16 C11 N2 . . 118.6(3)
C13 C12 C11 . . 120.1(4)
C13 C12 H12 . . 120.0
C11 C12 H12 . . 120.0
C14 C13 C12 . . 121.0(4)
C14 C13 H13 . . 119.5
C12 C13 H13 . . 119.5
C13 C14 C15 . . 119.6(4)
C13 C14 H14 . . 120.2
C15 C14 H14 . . 120.2
C14 C15 C16 . . 120.3(4)
C14 C15 H15 . . 119.9
C16 C15 H15 . . 119.9
C15 C16 C11 . . 120.1(4)
C15 C16 H16 . . 119.9
C11 C16 H16 . . 119.9
N3 C17 C18 . . 178.5(7)
C23 C18 C19 . . 119.0(5)
C23 C18 C17 . . 120.9(5)
C19 C18 C17 . . 120.0(5)
C20 C19 C18 . . 121.6(5)
C20 C19 H19 . . 119.2
C18 C19 H19 . . 119.2
C19 C20 C21 . . 118.1(6)
C19 C20 C24 . . 121.1(6)
C21 C20 C24 . . 120.8(5)
C22 C21 C20 . . 121.5(5)
C22 C21 H21 . . 119.2
C20 C21 H21 . . 119.2
C23 C22 C21 . . 120.6(5)
C23 C22 H22 . . 119.7
C21 C22 H22 . . 119.7
C22 C23 C18 . . 119.2(5)
C22 C23 H23 . . 120.4
C18 C23 H23 . . 120.4
C20 C24 H24A . . 109.5
C20 C24 H24B . . 109.5
H24A C24 H24B . . 109.5
C20 C24 H24C . . 109.5
H24A C24 H24C . . 109.5
H24B C24 H24C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Rh1 N1 . 2.053(3)
Rh1 N1 3 2.053(3)
Rh1 O2 3 2.058(2)
Rh1 O2 . 2.058(2)
Rh1 N3 . 2.177(4)
Rh1 Rh2 . 2.4086(6)
Rh2 N2 3 2.032(3)
Rh2 N2 . 2.032(3)
Rh2 O1 . 2.048(2)
Rh2 O1 3 2.048(2)
O1 C1 . 1.288(4)
O2 C3 . 1.290(4)
N1 C1 . 1.308(5)
N1 C5 . 1.431(5)
N2 C3 . 1.304(5)
N2 C11 . 1.434(4)
N3 C17 . 1.154(7)
C1 C2 . 1.511(5)
C2 H2A . 0.9700
C2 H2B . 0.9700
C2 H2C . 0.9700
C3 C4 . 1.503(5)
C4 H4A . 0.9700
C4 H4B . 0.9700
C4 H4C . 0.9700
C5 C6 . 1.370(5)
C5 C10 . 1.387(5)
C6 C7 . 1.392(5)
C6 H6 . 0.9400
C7 C8 . 1.370(6)
C7 H7 . 0.9400
C8 C9 . 1.380(6)
C8 H8 . 0.9400
C9 C10 . 1.385(6)
C9 H9 . 0.9400
C10 H10 . 0.9400
C11 C12 . 1.387(5)
C11 C16 . 1.394(5)
C12 C13 . 1.384(5)
C12 H12 . 0.9400
C13 C14 . 1.371(6)
C13 H13 . 0.9400
C14 C15 . 1.378(6)
C14 H14 . 0.9400
C15 C16 . 1.389(5)
C15 H15 . 0.9400
C16 H16 . 0.9400
C17 C18 . 1.444(8)
C18 C23 . 1.385(7)
C18 C19 . 1.411(8)
C19 C20 . 1.356(8)
C19 H19 . 0.9400
C20 C21 . 1.381(8)
C20 C24 . 1.513(8)
C21 C22 . 1.375(8)
C21 H21 . 0.9400
C22 C23 . 1.372(8)
C22 H22 . 0.9400
C23 H23 . 0.9400
C24 H24A . 0.9700
C24 H24B . 0.9700
C24 H24C . 0.9700
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
Rh2 O1 C1 N1 8.4(5)
Rh2 O1 C1 C2 -170.2(2)
C5 N1 C1 O1 -178.2(3)
Rh1 N1 C1 O1 -6.1(5)
C5 N1 C1 C2 0.3(5)
Rh1 N1 C1 C2 172.4(3)
Rh1 O2 C3 N2 -4.4(5)
Rh1 O2 C3 C4 174.4(2)
C11 N2 C3 O2 179.1(3)
Rh2 N2 C3 O2 3.6(5)
C11 N2 C3 C4 0.4(5)
Rh2 N2 C3 C4 -175.1(3)
C1 N1 C5 C6 -82.5(5)
Rh1 N1 C5 C6 105.1(4)
C1 N1 C5 C10 101.5(4)
Rh1 N1 C5 C10 -70.9(4)
C10 C5 C6 C7 -0.4(6)
N1 C5 C6 C7 -176.4(4)
C5 C6 C7 C8 0.5(7)
C6 C7 C8 C9 0.1(7)
C7 C8 C9 C10 -0.9(7)
C8 C9 C10 C5 1.1(7)
C6 C5 C10 C9 -0.4(6)
N1 C5 C10 C9 175.7(4)
C3 N2 C11 C12 61.3(5)
Rh2 N2 C11 C12 -122.9(3)
C3 N2 C11 C16 -121.2(4)
Rh2 N2 C11 C16 54.6(4)
C16 C11 C12 C13 2.6(6)
N2 C11 C12 C13 -179.9(4)
C11 C12 C13 C14 -1.3(7)
C12 C13 C14 C15 -0.8(7)
C13 C14 C15 C16 1.4(7)
C14 C15 C16 C11 -0.1(6)
C12 C11 C16 C15 -1.9(6)
N2 C11 C16 C15 -179.5(4)
C23 C18 C19 C20 0.0000(10)
C17 C18 C19 C20 180.0000(10)
C18 C19 C20 C21 0.0000(10)
C18 C19 C20 C24 180.0000(10)
C19 C20 C21 C22 0.0000(10)
C24 C20 C21 C22 180.0000(10)
C20 C21 C22 C23 0.0000(10)
C21 C22 C23 C18 0.0000(10)
C19 C18 C23 C22 0.0000(10)
C17 C18 C23 C22 180.0000(10)
