#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:34:00 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179796 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/92/7009207.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_7009207
loop_
_publ_author_name
'Coe, Benjamin J.'
'Beyer, Tim'
'Jeffery, John C.'
'Coles, Simon J.'
'Gelbrich, Thomas'
'Hursthouse, Michael B.'
'Light, Mark E.'
_publ_section_title
;
 A spectroscopic, electrochemical and structural study of polarizable,
 dipolar ruthenium(II) arsine complexes as models for chromophores with
 large quadratic non-linear optical responses
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              797
_journal_paper_doi               10.1039/a909336b
_journal_year                    2000
_chemical_formula_sum            'C30 H40 As4 Cl F6 N2 P Ru'
_chemical_formula_weight         1009.81
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.44(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.847(4)
_cell_length_b                   9.386(2)
_cell_length_c                   27.936(6)
_cell_measurement_temperature    293(2)
_cell_volume                     4586.6(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_sigmaI/netI    0.1205
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18799
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    3.342
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1984
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5811
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      3.438
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          2.506
_refine_ls_shift/su_mean         0.089
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1881
_reflns_number_gt                3558
_reflns_number_total             5811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909336b.txt
_cod_data_source_block           1
_cod_original_cell_volume        4586.6(17)
_cod_database_code               7009207
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.2578(2) 0.1201(3) 0.11244(15) 0.0314(13) Uani 1 1 d . . .
As1 As 0.1403(3) 0.2530(5) 0.0868(2) 0.0441(18) Uani 1 1 d . . .
As2 As 0.2209(3) 0.0042(4) 0.03387(19) 0.0326(15) Uani 1 1 d . . .
As3 As 0.3669(3) -0.0324(4) 0.14146(18) 0.0310(15) Uani 1 1 d . . .
As4 As 0.2858(3) 0.2228(4) 0.1931(2) 0.0446(17) Uani 1 1 d . . .
Cl1 Cl 0.1829(8) -0.0576(11) 0.1471(5) 0.048(4) Uani 1 1 d . . .
P1 P 0.1784(11) 0.5262(18) -0.0923(7) 0.074(5) Uani 1 1 d . . .
F1 F 0.247(2) 0.630(4) -0.0736(15) 0.107(13) Uani 1 1 d U . .
F2 F 0.240(3) 0.408(6) -0.0892(19) 0.184(19) Uani 1 1 d U . .
F3 F 0.184(3) 0.566(5) -0.1471(15) 0.131(15) Uani 1 1 d U . .
F4 F 0.112(4) 0.427(6) -0.110(2) 0.205(18) Uani 1 1 d U . .
F5 F 0.124(3) 0.654(5) -0.0957(18) 0.151(17) Uani 1 1 d U . .
F6 F 0.173(2) 0.499(4) -0.0360(14) 0.097(12) Uani 1 1 d U . .
N1 N 0.324(2) 0.273(3) 0.0857(14) 0.027(9) Uani 1 1 d . . .
N2 N 0.542(2) 0.832(4) 0.0060(18) 0.046(12) Uani 1 1 d . . .
C1 C 0.138(3) 0.459(4) 0.081(2) 0.056(17) Uani 1 1 d . . .
H1A H 0.1706 0.4884 0.0593 0.084 Uiso 1 1 calc R . .
H1B H 0.1570 0.5005 0.1129 0.084 Uiso 1 1 calc R . .
H1C H 0.0871 0.4905 0.0691 0.084 Uiso 1 1 calc R . .
C2 C 0.058(3) 0.227(5) 0.123(2) 0.07(2) Uani 1 1 d . . .
H2A H 0.0705 0.2763 0.1540 0.111 Uiso 1 1 calc R . .
H2B H 0.0512 0.1276 0.1290 0.111 Uiso 1 1 calc R . .
H2C H 0.0110 0.2654 0.1046 0.111 Uiso 1 1 calc R . .
C3 C 0.092(3) 0.194(5) 0.021(2) 0.046(15) Uani 1 1 d . . .
C4 C 0.025(3) 0.259(6) -0.006(3) 0.07(2) Uani 1 1 d . . .
H4 H 0.0018 0.3328 0.0081 0.083 Uiso 1 1 calc R . .
C5 C -0.005(4) 0.213(7) -0.052(3) 0.08(2) Uani 1 1 d . . .
H5 H -0.0510 0.2515 -0.0684 0.098 Uiso 1 1 calc R . .
C6 C 0.031(4) 0.108(6) -0.075(3) 0.08(2) Uani 1 1 d . . .
H6 H 0.0139 0.0862 -0.1075 0.094 Uiso 1 1 calc R . .
C7 C 0.092(3) 0.040(5) -0.048(3) 0.058(18) Uani 1 1 d . . .
H7 H 0.1133 -0.0378 -0.0615 0.070 Uiso 1 1 calc R . .
C8 C 0.124(3) 0.086(5) 0.000(2) 0.038(13) Uani 1 1 d . . .
C9 C 0.282(3) 0.018(4) -0.0160(18) 0.046(15) Uani 1 1 d . . .
H9A H 0.3351 0.0151 -0.0010 0.069 Uiso 1 1 calc R . .
H9B H 0.2707 0.1060 -0.0334 0.069 Uiso 1 1 calc R . .
H9C H 0.2700 -0.0604 -0.0383 0.069 Uiso 1 1 calc R . .
C10 C 0.199(3) -0.196(4) 0.0335(19) 0.046(15) Uani 1 1 d . . .
H10A H 0.1641 -0.2205 0.0040 0.069 Uiso 1 1 calc R . .
H10B H 0.1775 -0.2199 0.0612 0.069 Uiso 1 1 calc R . .
H10C H 0.2460 -0.2489 0.0350 0.069 Uiso 1 1 calc R . .
C11 C 0.461(3) -0.024(5) 0.1155(19) 0.046(14) Uani 1 1 d . . .
H11A H 0.4816 0.0707 0.1193 0.069 Uiso 1 1 calc R . .
H11B H 0.4501 -0.0490 0.0815 0.069 Uiso 1 1 calc R . .
H11C H 0.4978 -0.0898 0.1330 0.069 Uiso 1 1 calc R . .
C12 C 0.354(3) -0.239(4) 0.1420(18) 0.042(14) Uani 1 1 d . . .
H12A H 0.3978 -0.2815 0.1627 0.062 Uiso 1 1 calc R . .
H12B H 0.3491 -0.2754 0.1094 0.062 Uiso 1 1 calc R . .
H12C H 0.3089 -0.2621 0.1543 0.062 Uiso 1 1 calc R . .
C13 C 0.406(3) 0.007(4) 0.2111(17) 0.035(13) Uani 1 1 d . . .
C14 C 0.470(3) -0.065(5) 0.2375(18) 0.046(15) Uani 1 1 d . . .
H14 H 0.4946 -0.1337 0.2222 0.056 Uiso 1 1 calc R . .
C15 C 0.496(3) -0.035(6) 0.285(2) 0.058(16) Uani 1 1 d . . .
H15 H 0.5374 -0.0837 0.3032 0.069 Uiso 1 1 calc R . .
C16 C 0.458(4) 0.076(7) 0.308(2) 0.066(18) Uani 1 1 d . . .
H16 H 0.4776 0.1007 0.3401 0.079 Uiso 1 1 calc R . .
C17 C 0.395(4) 0.146(6) 0.283(2) 0.060(17) Uani 1 1 d . . .
H17 H 0.3698 0.2132 0.2990 0.072 Uiso 1 1 calc R . .
C18 C 0.368(3) 0.114(5) 0.234(2) 0.044(14) Uani 1 1 d . . .
C19 C 0.210(4) 0.229(5) 0.232(2) 0.08(2) Uani 1 1 d . . .
H19A H 0.2325 0.2098 0.2651 0.113 Uiso 1 1 calc R . .
H19B H 0.1712 0.1588 0.2202 0.113 Uiso 1 1 calc R . .
H19C H 0.1866 0.3219 0.2292 0.113 Uiso 1 1 calc R . .
C20 C 0.328(5) 0.417(5) 0.204(2) 0.10(3) Uani 1 1 d . . .
H20A H 0.3250 0.4473 0.2368 0.151 Uiso 1 1 calc R . .
H20B H 0.2986 0.4813 0.1811 0.151 Uiso 1 1 calc R . .
H20C H 0.3801 0.4176 0.2007 0.151 Uiso 1 1 calc R . .
C21 C 0.393(3) 0.315(4) 0.1109(18) 0.033(12) Uani 1 1 d . . .
H21 H 0.4114 0.2694 0.1405 0.039 Uiso 1 1 calc R . .
C22 C 0.437(3) 0.420(5) 0.0962(18) 0.042(13) Uani 1 1 d . . .
H22 H 0.4854 0.4412 0.1148 0.050 Uiso 1 1 calc R . .
C23 C 0.410(3) 0.492(4) 0.0536(17) 0.028(12) Uani 1 1 d . . .
C24 C 0.340(3) 0.455(4) 0.0260(17) 0.029(12) Uani 1 1 d . . .
H24 H 0.3211 0.5023 -0.0031 0.035 Uiso 1 1 calc R . .
C25 C 0.299(3) 0.344(4) 0.0424(17) 0.030(12) Uani 1 1 d . . .
H25 H 0.2522 0.3178 0.0232 0.036 Uiso 1 1 calc R . .
C26 C 0.532(3) 0.637(4) 0.0608(18) 0.041(14) Uani 1 1 d . . .
H26 H 0.5551 0.5829 0.0876 0.049 Uiso 1 1 calc R . .
C27 C 0.573(3) 0.747(5) 0.043(2) 0.047(15) Uani 1 1 d . . .
H27 H 0.6235 0.7613 0.0577 0.057 Uiso 1 1 calc R . .
C28 C 0.457(3) 0.612(4) 0.0370(19) 0.035(13) Uani 1 1 d . . .
C29 C 0.469(3) 0.806(4) -0.016(2) 0.045(15) Uani 1 1 d . . .
H29 H 0.4477 0.8639 -0.0420 0.054 Uiso 1 1 calc R . .
C30 C 0.424(3) 0.698(4) -0.0019(19) 0.042(14) Uani 1 1 d . . .
H30 H 0.3737 0.6839 -0.0180 0.051 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
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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 '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'
Ru Ru -1.2594 0.8363 '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
N1 Ru1 As4 91.8(10) . . ?
N1 Ru1 As2 93.3(10) . . ?
As4 Ru1 As2 174.8(2) . . ?
N1 Ru1 As3 92.9(10) . . ?
As4 Ru1 As3 85.4(2) . . ?
As2 Ru1 As3 95.4(2) . . ?
N1 Ru1 As1 93.5(10) . . ?
As4 Ru1 As1 94.4(2) . . ?
As2 Ru1 As1 84.2(2) . . ?
As3 Ru1 As1 173.6(2) . . ?
N1 Ru1 Cl1 177.6(12) . . ?
As4 Ru1 Cl1 86.0(4) . . ?
As2 Ru1 Cl1 88.9(4) . . ?
As3 Ru1 Cl1 86.0(3) . . ?
As1 Ru1 Cl1 87.6(3) . . ?
C1 As1 C3 102(2) . . ?
C1 As1 C2 99(2) . . ?
C3 As1 C2 103(3) . . ?
C1 As1 Ru1 122.4(16) . . ?
C3 As1 Ru1 108.9(15) . . ?
C2 As1 Ru1 118.6(16) . . ?
C10 As2 C9 101.6(19) . . ?
C10 As2 C8 103(2) . . ?
C9 As2 C8 101(2) . . ?
C10 As2 Ru1 117.6(15) . . ?
C9 As2 Ru1 122.1(14) . . ?
C8 As2 Ru1 108.7(16) . . ?
C12 As3 C11 98.8(19) . . ?
C12 As3 C13 101.4(19) . . ?
C11 As3 C13 101(2) . . ?
C12 As3 Ru1 120.1(15) . . ?
C11 As3 Ru1 122.9(15) . . ?
C13 As3 Ru1 108.8(14) . . ?
C19 As4 C18 103(2) . . ?
C19 As4 C20 100(3) . . ?
C18 As4 C20 100(3) . . ?
C19 As4 Ru1 120(2) . . ?
C18 As4 Ru1 108.9(14) . . ?
C20 As4 Ru1 121.3(17) . . ?
F4 P1 F5 91(3) . . ?
F4 P1 F2 95(4) . . ?
F5 P1 F2 174(4) . . ?
F4 P1 F1 180(4) . . ?
F5 P1 F1 89(3) . . ?
F2 P1 F1 86(3) . . ?
F4 P1 F3 91(3) . . ?
F5 P1 F3 86(3) . . ?
F2 P1 F3 92(3) . . ?
F1 P1 F3 89(2) . . ?
F4 P1 F6 92(3) . . ?
F5 P1 F6 91(3) . . ?
F2 P1 F6 91(3) . . ?
F1 P1 F6 88(2) . . ?
F3 P1 F6 176(3) . . ?
C21 N1 C25 116(4) . . ?
C21 N1 Ru1 122(3) . . ?
C25 N1 Ru1 122(3) . . ?
C29 N2 C27 117(4) . . ?
C8 C3 C4 119(6) . . ?
C8 C3 As1 118(4) . . ?
C4 C3 As1 122(5) . . ?
C5 C4 C3 119(6) . . ?
C4 C5 C6 121(6) . . ?
C7 C6 C5 119(7) . . ?
C6 C7 C8 120(6) . . ?
C3 C8 C7 120(5) . . ?
C3 C8 As2 120(4) . . ?
C7 C8 As2 120(4) . . ?
C14 C13 C18 121(5) . . ?
C14 C13 As3 121(3) . . ?
C18 C13 As3 118(4) . . ?
C15 C14 C13 120(5) . . ?
C14 C15 C16 119(6) . . ?
C17 C16 C15 122(6) . . ?
C16 C17 C18 118(5) . . ?
C17 C18 C13 120(5) . . ?
C17 C18 As4 122(4) . . ?
C13 C18 As4 119(4) . . ?
N1 C21 C22 125(4) . . ?
C23 C22 C21 119(5) . . ?
C24 C23 C22 120(4) . . ?
C24 C23 C28 121(4) . . ?
C22 C23 C28 120(5) . . ?
C23 C24 C25 119(4) . . ?
N1 C25 C24 123(4) . . ?
C27 C26 C28 118(5) . . ?
N2 C27 C26 123(5) . . ?
C30 C28 C26 120(4) . . ?
C30 C28 C23 119(4) . . ?
C26 C28 C23 121(4) . . ?
N2 C29 C30 124(5) . . ?
C28 C30 C29 117(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
Ru1 N1 2.10(3) . ?
Ru1 As4 2.410(7) . ?
Ru1 As2 2.421(6) . ?
Ru1 As3 2.423(6) . ?
Ru1 As1 2.424(6) . ?
Ru1 Cl1 2.455(12) . ?
As1 C1 1.94(4) . ?
As1 C3 1.96(5) . ?
As1 C2 1.97(5) . ?
As2 C10 1.92(4) . ?
As2 C9 1.93(5) . ?
As2 C8 1.95(5) . ?
As3 C12 1.95(4) . ?
As3 C11 1.96(5) . ?
As3 C13 1.97(5) . ?
As4 C19 1.90(6) . ?
As4 C18 1.96(5) . ?
As4 C20 1.97(5) . ?
P1 F4 1.52(5) . ?
P1 F5 1.54(4) . ?
P1 F2 1.56(5) . ?
P1 F1 1.57(4) . ?
P1 F3 1.60(4) . ?
P1 F6 1.61(4) . ?
N1 C21 1.34(5) . ?
N1 C25 1.38(5) . ?
N2 C29 1.33(6) . ?
N2 C27 1.34(6) . ?
C3 C8 1.35(7) . ?
C3 C4 1.42(7) . ?
C4 C5 1.36(8) . ?
C5 C6 1.40(8) . ?
C6 C7 1.35(8) . ?
C7 C8 1.42(7) . ?
C13 C14 1.41(7) . ?
C13 C18 1.42(6) . ?
C14 C15 1.35(7) . ?
C15 C16 1.45(8) . ?
C16 C17 1.37(8) . ?
C17 C18 1.41(7) . ?
C21 C22 1.38(6) . ?
C22 C23 1.37(6) . ?
C23 C24 1.37(6) . ?
C23 C28 1.53(6) . ?
C24 C25 1.41(6) . ?
C26 C27 1.40(6) . ?
C26 C28 1.40(6) . ?
C28 C30 1.39(6) . ?
C29 C30 1.40(6) . ?
