#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:09:19 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179525 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/22/4342228.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_4342228
loop_
_publ_author_name
'Choudhuri, Mohommad M. R.'
'Behzad, Mahdi'
'Al-Noaimi, Mousa'
'Yap, Glenn P. A.'
'Kaim, Wolfgang'
'Sarkar, Biprajit'
'Crutchley, Robert J.'
_publ_section_title
;
 Variable Noninnocence of Substituted Azobis(phenylcyanamido)diruthenium
 Complexes.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1508
_journal_page_last               1517
_journal_paper_doi               10.1021/ic502487x
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C32 H26 As N3'
_chemical_formula_weight         527.48
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   '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                 90.605(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.992(5)
_cell_length_b                   10.885(6)
_cell_length_c                   26.000(14)
_cell_measurement_reflns_used    1022
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.74
_cell_volume                     2545(2)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            26941
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.064
_diffrn_reflns_theta_min         2.028
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.6927
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.291
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0462P)²+0.7343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5181
_reflns_number_total             5774
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic502487x_si_002.cif
_cod_data_source_block           bobr003
_cod_depositor_comments          'Adding full bibliography for 4342228.cif.'
_cod_database_code               4342228
#BEGIN Tags that were not found in dictionaries:
_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   0.625
_shelx_estimated_absorpt_t_max   0.693
#END Tags that were not found in dictionaries
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
As As 0.33809(2) 0.59186(2) 0.33772(2) 0.01896(6) Uani 1 1 d . .
N1 N 0.83475(17) 1.10089(12) 0.36072(6) 0.0282(3) Uani 1 1 d . .
N2 N 0.78953(16) 0.87751(12) 0.35270(5) 0.0256(3) Uani 1 1 d . .
N3 N 0.98866(15) 0.55498(12) 0.50723(5) 0.0222(3) Uani 1 1 d . .
C1 C 0.81325(17) 0.99539(14) 0.35924(6) 0.0228(3) Uani 1 1 d . .
C2 C 0.82819(16) 0.79974(14) 0.39274(6) 0.0209(3) Uani 1 1 d . .
C3 C 0.86993(16) 0.83919(13) 0.44248(6) 0.0209(3) Uani 1 1 d . .
H3A H 0.8617 0.9240 0.4507 0.025 Uiso 1 1 calc R U
C4 C 0.92260(16) 0.75901(14) 0.47995(6) 0.0213(3) Uani 1 1 d . .
C5 C 0.93002(16) 0.63241(14) 0.46851(6) 0.0201(3) Uani 1 1 d . .
C6 C 0.87865(17) 0.59069(13) 0.42030(6) 0.0219(3) Uani 1 1 d . .
H6A H 0.8775 0.5051 0.4132 0.026 Uiso 1 1 calc R U
C7 C 0.83000(17) 0.67180(14) 0.38317(6) 0.0236(3) Uani 1 1 d . .
H7A H 0.7972 0.6415 0.3507 0.028 Uiso 1 1 calc R U
C8 C 0.9744(2) 0.80688(15) 0.53139(6) 0.0324(4) Uani 1 1 d . .
H8A H 0.9676 0.8967 0.5317 0.049 Uiso 1 1 calc R U
H8B H 1.0778 0.7820 0.5375 0.049 Uiso 1 1 calc R U
H8C H 0.9114 0.7731 0.5585 0.049 Uiso 1 1 calc R U
C9 C 0.46130(16) 0.61803(14) 0.27914(6) 0.0201(3) Uani 1 1 d . .
C10 C 0.57061(17) 0.70876(14) 0.28117(6) 0.0221(3) Uani 1 1 d . .
H10A H 0.5828 0.7584 0.3110 0.027 Uiso 1 1 calc R U
C11 C 0.66142(17) 0.72532(15) 0.23885(6) 0.0248(3) Uani 1 1 d . .
H11A H 0.7384 0.7851 0.2400 0.030 Uiso 1 1 calc R U
C12 C 0.64027(18) 0.65507(15) 0.19482(6) 0.0265(3) Uani 1 1 d . .
H12A H 0.7012 0.6686 0.1657 0.032 Uiso 1 1 calc R U
C13 C 0.53090(18) 0.56525(16) 0.19299(6) 0.0272(3) Uani 1 1 d . .
H13A H 0.5175 0.5171 0.1628 0.033 Uiso 1 1 calc R U
C14 C 0.44127(17) 0.54586(15) 0.23524(6) 0.0239(3) Uani 1 1 d . .
H14A H 0.3668 0.4840 0.2343 0.029 Uiso 1 1 calc R U
C15 C 0.15300(16) 0.52716(14) 0.31301(6) 0.0211(3) Uani 1 1 d . .
C16 C 0.09110(18) 0.57503(15) 0.26771(6) 0.0257(3) Uani 1 1 d . .
H16A H 0.1363 0.6429 0.2510 0.031 Uiso 1 1 calc R U
C17 C -0.03714(18) 0.52225(17) 0.24739(7) 0.0311(4) Uani 1 1 d . .
H17A H -0.0800 0.5539 0.2166 0.037 Uiso 1 1 calc R U
C18 C -0.10301(19) 0.42331(16) 0.27203(7) 0.0322(4) Uani 1 1 d . .
H18A H -0.1915 0.3883 0.2581 0.039 Uiso 1 1 calc R U
C19 C -0.04093(19) 0.37511(16) 0.31669(7) 0.0303(4) Uani 1 1 d . .
H19A H -0.0862 0.3069 0.3331 0.036 Uiso 1 1 calc R U
C20 C 0.08806(18) 0.42693(14) 0.33749(6) 0.0245(3) Uani 1 1 d . .
H20A H 0.1313 0.3943 0.3681 0.029 Uiso 1 1 calc R U
C21 C 0.42665(17) 0.47545(14) 0.38376(6) 0.0217(3) Uani 1 1 d . .
C22 C 0.54449(19) 0.40340(14) 0.36765(6) 0.0257(3) Uani 1 1 d . .
H22A H 0.5845 0.4138 0.3343 0.031 Uiso 1 1 calc R U
C23 C 0.6034(2) 0.31571(16) 0.40099(7) 0.0321(4) Uani 1 1 d . .
H23A H 0.6842 0.2657 0.3905 0.039 Uiso 1 1 calc R U
C24 C 0.5443(2) 0.30139(17) 0.44946(7) 0.0345(4) Uani 1 1 d . .
H24A H 0.5851 0.2414 0.4721 0.041 Uiso 1 1 calc R U
C25 C 0.4260(2) 0.37360(19) 0.46553(7) 0.0352(4) Uani 1 1 d . .
H25A H 0.3864 0.3629 0.4990 0.042 Uiso 1 1 calc R U
C26 C 0.36575(19) 0.46132(17) 0.43258(6) 0.0297(4) Uani 1 1 d . .
H26A H 0.2845 0.5108 0.4431 0.036 Uiso 1 1 calc R U
C27 C 0.32056(16) 0.74382(14) 0.37427(6) 0.0208(3) Uani 1 1 d . .
C28 C 0.44046(17) 0.77860(15) 0.40582(6) 0.0233(3) Uani 1 1 d . .
H28A H 0.5240 0.7259 0.4100 0.028 Uiso 1 1 calc R U
C29 C 0.43573(19) 0.89123(15) 0.43094(6) 0.0261(3) Uani 1 1 d . .
H29A H 0.5168 0.9165 0.4521 0.031 Uiso 1 1 calc R U
C30 C 0.31204(18) 0.96691(15) 0.42501(6) 0.0265(3) Uani 1 1 d . .
H30A H 0.3086 1.0434 0.4426 0.032 Uiso 1 1 calc R U
C31 C 0.19346(18) 0.93154(15) 0.39362(6) 0.0263(3) Uani 1 1 d . .
H31A H 0.1096 0.9839 0.3898 0.032 Uiso 1 1 calc R U
C32 C 0.19729(17) 0.81957(15) 0.36782(6) 0.0238(3) Uani 1 1 d . .
H32A H 0.1169 0.7953 0.3461 0.029 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'
As As 0.0499 2.0058 '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
C15 As C21 108.77(7) .
C15 As C27 114.14(7) .
C21 As C27 107.33(7) .
C15 As C9 107.24(7) .
C21 As C9 110.87(7) .
C27 As C9 108.52(7) .
C1 N2 C2 117.52(13) .
N3 N3 C5 114.28(16) 3_766
N1 C1 N2 174.45(17) .
N2 C2 C3 124.49(14) .
N2 C2 C7 118.25(14) .
C3 C2 C7 117.24(14) .
C4 C3 C2 122.55(14) .
C3 C4 C5 118.86(14) .
C3 C4 C8 120.42(14) .
C5 C4 C8 120.70(14) .
C6 C5 N3 124.04(14) .
C6 C5 C4 119.15(14) .
N3 C5 C4 116.81(14) .
C7 C6 C5 121.13(14) .
C6 C7 C2 120.81(14) .
C10 C9 C14 120.97(14) .
C10 C9 As 119.28(11) .
C14 C9 As 119.75(12) .
C11 C10 C9 118.82(14) .
C10 C11 C12 120.36(15) .
C13 C12 C11 120.49(15) .
C14 C13 C12 119.90(15) .
C13 C14 C9 119.44(15) .
C20 C15 C16 120.75(15) .
C20 C15 As 120.13(12) .
C16 C15 As 118.89(12) .
C17 C16 C15 119.22(16) .
C16 C17 C18 120.14(16) .
C19 C18 C17 120.66(16) .
C18 C19 C20 119.86(16) .
C15 C20 C19 119.36(16) .
C22 C21 C26 121.38(15) .
C22 C21 As 120.03(12) .
C26 C21 As 118.53(12) .
C21 C22 C23 119.16(16) .
C24 C23 C22 119.90(16) .
C23 C24 C25 120.86(16) .
C26 C25 C24 119.86(16) .
C25 C26 C21 118.84(16) .
C32 C27 C28 121.23(14) .
C32 C27 As 121.47(12) .
C28 C27 As 117.22(11) .
C29 C28 C27 119.12(15) .
C28 C29 C30 119.91(15) .
C31 C30 C29 120.56(15) .
C30 C31 C32 120.18(15) .
C27 C32 C31 119.01(15) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As C15 1.9120(17) .
As C21 1.9112(16) .
As C27 1.9150(17) .
As C9 1.9143(17) .
N1 C1 1.165(2) .
N2 C1 1.311(2) .
N2 C2 1.383(2) .
N3 N3 1.272(3) 3_766
N3 C5 1.411(2) .
C2 C3 1.410(2) .
C2 C7 1.415(2) .
C3 C4 1.388(2) .
C4 C5 1.412(2) .
C4 C8 1.505(2) .
C5 C6 1.407(2) .
C6 C7 1.376(2) .
C9 C10 1.394(2) .
C9 C14 1.396(2) .
C10 C11 1.389(2) .
C11 C12 1.388(2) .
C12 C13 1.387(2) .
C13 C14 1.385(2) .
C15 C20 1.394(2) .
C15 C16 1.398(2) .
C16 C17 1.388(2) .
C17 C18 1.389(3) .
C18 C19 1.386(3) .
C19 C20 1.394(2) .
C21 C22 1.387(2) .
C21 C26 1.396(2) .
C22 C23 1.391(2) .
C23 C24 1.382(3) .
C24 C25 1.391(3) .
C25 C26 1.389(2) .
C27 C32 1.390(2) .
C27 C28 1.400(2) .
C28 C29 1.390(2) .
C29 C30 1.391(2) .
C30 C31 1.390(2) .
C31 C32 1.392(2) .
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
C1 N2 C2 C3 10.0(2) .
C1 N2 C2 C7 -168.29(15) .
N2 C2 C3 C4 -173.16(15) .
C7 C2 C3 C4 5.2(2) .
C2 C3 C4 C5 -2.2(2) .
C2 C3 C4 C8 176.29(15) .
N3 N3 C5 C6 9.4(2) 3_766
N3 N3 C5 C4 -171.12(16) 3_766
C3 C4 C5 C6 -2.4(2) .
C8 C4 C5 C6 179.09(15) .
C3 C4 C5 N3 178.06(13) .
C8 C4 C5 N3 -0.4(2) .
N3 C5 C6 C7 -176.51(14) .
C4 C5 C6 C7 4.0(2) .
C5 C6 C7 C2 -1.0(2) .
N2 C2 C7 C6 174.91(14) .
C3 C2 C7 C6 -3.5(2) .
C14 C9 C10 C11 -0.9(2) .
As C9 C10 C11 178.70(11) .
C9 C10 C11 C12 1.9(2) .
C10 C11 C12 C13 -1.7(2) .
C11 C12 C13 C14 0.4(3) .
C12 C13 C14 C9 0.6(2) .
C10 C9 C14 C13 -0.3(2) .
As C9 C14 C13 -179.96(12) .
C20 C15 C16 C17 0.5(2) .
As C15 C16 C17 175.07(12) .
C15 C16 C17 C18 0.2(2) .
C16 C17 C18 C19 -0.8(3) .
C17 C18 C19 C20 0.6(3) .
C16 C15 C20 C19 -0.7(2) .
As C15 C20 C19 -175.17(12) .
C18 C19 C20 C15 0.1(2) .
C26 C21 C22 C23 -0.3(2) .
As C21 C22 C23 -177.37(13) .
C21 C22 C23 C24 0.0(3) .
C22 C23 C24 C25 0.1(3) .
C23 C24 C25 C26 0.1(3) .
C24 C25 C26 C21 -0.4(3) .
C22 C21 C26 C25 0.5(3) .
As C21 C26 C25 177.58(14) .
C32 C27 C28 C29 -0.2(2) .
As C27 C28 C29 176.67(11) .
C27 C28 C29 C30 0.8(2) .
C28 C29 C30 C31 -0.8(2) .
C29 C30 C31 C32 0.1(2) .
C28 C27 C32 C31 -0.5(2) .
As C27 C32 C31 -177.16(12) .
C30 C31 C32 C27 0.5(2) .
