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#$Date: 2016-03-26 19:24:35 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180433 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/02/7210285.cif $
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#
# 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_7210285
loop_
_publ_author_name
'Bacchi, Alessia'
'Cantoni, Giulia'
'Pelagatti, Paolo'
_publ_section_title
;
 Polymorphs and co-crystal with half-sandwich Ru(ii) dimers
 [(η6-arene)RuX2]2
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              6722
_journal_paper_doi               10.1039/c3ce40618k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C18 H23 Cl2 N O2 Ru'
_chemical_formula_weight         457.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                90.000(5)
_cell_angle_beta                 112.476(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   15.659(5)
_cell_length_b                   7.660(5)
_cell_length_c                   17.820(5)
_cell_measurement_reflns_used    5280
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      47.12
_cell_measurement_theta_min      4.401
_cell_volume                     1975.1(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Altomare et al. 2004)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  diffractometer
_diffrn_measurement_method       'ω scan'
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29577
_diffrn_reflns_theta_full        29.87
_diffrn_reflns_theta_max         29.87
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.074
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS procedure'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         5673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0311P)²+0.3650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                4204
_reflns_number_total             5673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40618k.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7210285
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
Ru1 Ru 0.117943(13) -0.44553(2) 0.507979(11) 0.03084(7) Uani 1 1 d .
Cl1 Cl 0.02414(5) -0.42785(9) 0.59020(4) 0.04387(16) Uani 1 1 d .
Cl2 Cl 0.15839(6) -0.73527(9) 0.56074(5) 0.0591(2) Uani 1 1 d .
N1 N 0.2753(3) 0.0996(5) 0.4509(2) 0.0705(9) Uani 1 1 d .
O2 O 0.10137(17) -0.0530(3) 0.07270(15) 0.0764(7) Uani 1 1 d .
H2A H 0.0641 -0.0546 0.0255 0.115 Uiso 1 1 calc R
O1 O -0.01468(17) 0.0933(4) 0.08541(15) 0.0797(7) Uani 1 1 d .
C5 C 0.26130(18) -0.3918(4) 0.53677(16) 0.0441(6) Uani 1 1 d .
H5 H 0.3132 -0.4594 0.5644 0.053 Uiso 1 1 calc R
C8 C 0.2738(2) -0.2538(4) 0.67248(17) 0.0534(7) Uani 1 1 d .
H8 H 0.2238 -0.2406 0.6924 0.064 Uiso 1 1 calc R
C1 C 0.13818(18) -0.3105(4) 0.40794(16) 0.0438(6) Uani 1 1 d .
C3 C 0.1496(2) -0.1748(3) 0.53601(18) 0.0446(6) Uani 1 1 d .
H3 H 0.1262 -0.0967 0.5633 0.054 Uiso 1 1 calc R
C16 C 0.1364(2) 0.1506(4) 0.3350(2) 0.0596(8) Uani 1 1 d .
H16 H 0.1112 0.2080 0.3678 0.072 Uiso 1 1 calc R
C14 C 0.1212(2) 0.0488(4) 0.2019(2) 0.0525(7) Uani 1 1 d .
C4 C 0.22967(17) -0.2746(4) 0.58116(16) 0.0411(6) Uani 1 1 d .
C17 C 0.0677(2) 0.0288(4) 0.1158(2) 0.0564(8) Uani 1 1 d .
C15 C 0.0852(2) 0.1345(4) 0.2536(2) 0.0570(8) Uani 1 1 d .
H15 H 0.0258 0.1808 0.2320 0.068 Uiso 1 1 calc R
C11 C 0.2261(2) 0.0819(4) 0.3700(2) 0.0551(8) Uani 1 1 d .
C7 C 0.0877(2) -0.3376(5) 0.31828(16) 0.0596(8) Uani 1 1 d .
H7A H 0.1203 -0.4215 0.2993 0.089 Uiso 1 1 calc R
H7B H 0.0840 -0.2288 0.2904 0.089 Uiso 1 1 calc R
H7C H 0.0264 -0.3797 0.3079 0.089 Uiso 1 1 calc R
C6 C 0.21684(19) -0.4106(4) 0.45129(16) 0.0437(6) Uani 1 1 d .
H6 H 0.2398 -0.4893 0.4239 0.052 Uiso 1 1 calc R
C2 C 0.1050(2) -0.1915(3) 0.45132(17) 0.0464(7) Uani 1 1 d .
H2 H 0.0533 -0.1236 0.4235 0.056 Uiso 1 1 calc R
C12 C 0.2613(2) -0.0036(4) 0.3186(2) 0.0596(8) Uani 1 1 d .
H12 H 0.3207 -0.0499 0.3399 0.072 Uiso 1 1 calc R
C10 C 0.3305(3) -0.0863(4) 0.6926(2) 0.0729(11) Uani 1 1 d .
H10A H 0.3585 -0.0723 0.7505 0.109 Uiso 1 1 calc R
H10B H 0.2909 0.0115 0.6692 0.109 Uiso 1 1 calc R
H10C H 0.3778 -0.0926 0.6709 0.109 Uiso 1 1 calc R
C13 C 0.2094(2) -0.0196(4) 0.2375(2) 0.0563(8) Uani 1 1 d .
H13 H 0.2342 -0.0787 0.2049 0.068 Uiso 1 1 calc R
C18 C 0.3675(3) 0.0333(6) 0.4918(2) 0.0852(13) Uani 1 1 d .
H18A H 0.3888 0.0609 0.5486 0.128 Uiso 1 1 calc R
H18B H 0.4079 0.0857 0.4690 0.128 Uiso 1 1 calc R
H18C H 0.3674 -0.0911 0.4851 0.128 Uiso 1 1 calc R
C9 C 0.3317(3) -0.4099(5) 0.7157(2) 0.0774(11) Uani 1 1 d .
H9A H 0.3576 -0.3887 0.7731 0.116 Uiso 1 1 calc R
H9B H 0.3807 -0.4274 0.6966 0.116 Uiso 1 1 calc R
H9C H 0.2935 -0.5123 0.7046 0.116 Uiso 1 1 calc R
H1N H 0.251(2) 0.138(5) 0.475(2) 0.056(12) Uiso 1 1 d .
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'
Cl Cl 0.1484 0.1585 '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_3
C5 Ru1 C3 68.37(11) .
C5 Ru1 C6 38.48(10) .
C3 Ru1 C6 81.17(11) .
C5 Ru1 C2 80.89(11) .
C3 Ru1 C2 38.04(11) .
C6 Ru1 C2 68.13(11) .
C5 Ru1 C4 37.99(10) .
C3 Ru1 C4 38.53(11) .
C6 Ru1 C4 69.54(10) .
C2 Ru1 C4 69.45(11) .
C5 Ru1 C1 68.85(10) .
C3 Ru1 C1 68.91(11) .
C6 Ru1 C1 37.67(10) .
C2 Ru1 C1 37.98(11) .
C4 Ru1 C1 82.53(10) .
C5 Ru1 Cl2 89.33(8) .
C3 Ru1 Cl2 143.11(9) .
C6 Ru1 Cl2 99.70(8) .
C2 Ru1 Cl2 167.83(8) .
C4 Ru1 Cl2 106.89(8) .
C1 Ru1 Cl2 131.18(8) .
C5 Ru1 Cl1 131.36(8) .
C3 Ru1 Cl1 86.85(8) .
C6 Ru1 Cl1 167.01(8) .
C2 Ru1 Cl1 105.03(8) .
C4 Ru1 Cl1 97.89(7) .
C1 Ru1 Cl1 140.41(8) .
Cl2 Ru1 Cl1 86.87(3) .
C5 Ru1 Cl1 146.22(8) 3_546
C3 Ru1 Cl1 128.01(8) 3_546
C6 Ru1 Cl1 109.44(8) 3_546
C2 Ru1 Cl1 97.22(8) 3_546
C4 Ru1 Cl1 166.24(8) 3_546
C1 Ru1 Cl1 88.86(7) 3_546
Cl2 Ru1 Cl1 86.85(4) 3_546
Cl1 Ru1 Cl1 81.94(3) 3_546
Ru1 Cl1 Ru1 98.06(3) 3_546
C11 N1 C18 123.8(4) .
C4 C5 C6 122.3(3) .
C4 C5 Ru1 72.25(15) .
C6 C5 Ru1 71.61(15) .
C4 C8 C9 113.6(3) .
C4 C8 C10 109.1(3) .
C9 C8 C10 111.2(3) .
C6 C1 C2 118.6(2) .
C6 C1 C7 120.3(3) .
C2 C1 C7 121.1(3) .
C6 C1 Ru1 70.33(15) .
C2 C1 Ru1 70.23(15) .
C7 C1 Ru1 128.36(19) .
C2 C3 C4 121.7(3) .
C2 C3 Ru1 71.75(15) .
C4 C3 Ru1 71.84(15) .
C15 C16 C11 121.2(3) .
C13 C14 C15 117.1(3) .
C13 C14 C17 121.1(3) .
C15 C14 C17 121.8(3) .
C5 C4 C3 116.6(2) .
C5 C4 C8 123.9(3) .
C3 C4 C8 119.4(3) .
C5 C4 Ru1 69.75(15) .
C3 C4 Ru1 69.63(15) .
C8 C4 Ru1 129.77(19) .
O2 C17 O1 121.5(3) .
O2 C17 C14 119.6(3) .
O1 C17 C14 118.9(3) .
C16 C15 C14 121.0(3) .
N1 C11 C12 122.4(4) .
N1 C11 C16 120.0(3) .
C12 C11 C16 117.6(3) .
C1 C6 C5 120.1(3) .
C1 C6 Ru1 72.00(15) .
C5 C6 Ru1 69.92(15) .
C3 C2 C1 120.6(3) .
C3 C2 Ru1 70.21(15) .
C1 C2 Ru1 71.79(15) .
C13 C12 C11 120.7(3) .
C12 C13 C14 122.4(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C5 2.143(3) .
Ru1 C3 2.146(3) .
Ru1 C6 2.165(3) .
Ru1 C2 2.166(3) .
Ru1 C4 2.175(3) .
Ru1 C1 2.186(3) .
Ru1 Cl2 2.3991(15) .
Ru1 Cl1 2.4430(8) .
Ru1 Cl1 2.4444(9) 3_546
Cl1 Ru1 2.4444(8) 3_546
N1 C11 1.357(4) .
N1 C18 1.438(5) .
O2 C17 1.253(4) .
O1 C17 1.291(4) .
C5 C4 1.406(4) .
C5 C6 1.419(4) .
C8 C4 1.514(4) .
C8 C9 1.521(5) .
C8 C10 1.523(4) .
C1 C6 1.405(4) .
C1 C2 1.416(4) .
C1 C7 1.502(4) .
C3 C2 1.405(4) .
C3 C4 1.426(4) .
C16 C15 1.368(4) .
C16 C11 1.403(5) .
C14 C13 1.383(4) .
C14 C15 1.413(4) .
C14 C17 1.449(5) .
C11 C12 1.399(4) .
C12 C13 1.367(4) .
