data_pccn
 
#Dr. N. Fletcher

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C20 H28 B Cl3 F4 Ru2'
_chemical_formula_weight          663.72
 
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'
 'B'  'B'   0.0013   0.0007
 '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'
 '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'
 
_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    Pccn
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y+1/2, z'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y-1/2, -z'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y, z-1/2'
 
_cell_length_a                    10.7827(12)
_cell_length_b                    13.1678(12)
_cell_length_c                    16.8284(18)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      2389.4(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3661
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        shard
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.16
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.845
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1312
_exptl_absorpt_coefficient_mu     1.636
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7798
_exptl_absorpt_correction_T_max   0.9680
_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Parameter refinement on 16919 reflections reduced R(int) from 0.1266 to 0.0657
Ratio of minimum to maximum apparent transmission: 0.538150
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type   
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             20802
_diffrn_reflns_av_R_equivalents   0.0786
_diffrn_reflns_av_sigmaI/netI     0.0511
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          3.07
_diffrn_reflns_theta_max          27.48
_reflns_number_total              2732
_reflns_number_gt                 1986
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX (Farrugia, 1999)'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0412P)²+28.7650P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          2732
_refine_ls_number_parameters      157
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0930
_refine_ls_R_factor_gt            0.0606
_refine_ls_wR_factor_ref          0.1486
_refine_ls_wR_factor_gt           0.1276
_refine_ls_goodness_of_fit_ref    1.092
_refine_ls_restrained_S_all       1.092
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
C1 C 0.1002(7) 0.5322(5) 0.2115(4) 0.0272(15) Uani 1 1 d . . .
C2 C 0.1526(7) 0.4913(5) 0.2826(4) 0.0277(15) Uani 1 1 d . . .
H2 H 0.2179 0.4431 0.2788 0.033 Uiso 1 1 calc R . .
C3 C 0.1102(7) 0.5204(5) 0.3574(4) 0.0299(16) Uani 1 1 d . . .
H3 H 0.1487 0.4936 0.4036 0.036 Uiso 1 1 calc R . .
C4 C 0.0099(7) 0.5898(5) 0.3654(4) 0.0280(16) Uani 1 1 d . . .
C5 C -0.0447(7) 0.6287(5) 0.2955(4) 0.0259(15) Uani 1 1 d . . .
H5 H -0.1129 0.6742 0.2994 0.031 Uiso 1 1 calc R . .
C6 C 0.0011(7) 0.6007(5) 0.2193(5) 0.0298(16) Uani 1 1 d . . .
H6 H -0.0358 0.6288 0.1730 0.036 Uiso 1 1 calc R . .
C7 C 0.1561(8) 0.5034(5) 0.1320(4) 0.0300(16) Uani 1 1 d . . .
H7 H 0.2480 0.4996 0.1395 0.036 Uiso 1 1 calc R . .
C8 C 0.1320(9) 0.5791(6) 0.0660(5) 0.045(2) Uani 1 1 d . . .
H8A H 0.0428 0.5822 0.0551 0.067 Uiso 1 1 calc R . .
H8B H 0.1762 0.5578 0.0179 0.067 Uiso 1 1 calc R . .
H8C H 0.1614 0.6464 0.0824 0.067 Uiso 1 1 calc R . .
C9 C 0.1117(9) 0.3966(6) 0.1088(5) 0.042(2) Uani 1 1 d . . .
H9A H 0.0209 0.3956 0.1066 0.063 Uiso 1 1 calc R . .
H9B H 0.1403 0.3474 0.1485 0.063 Uiso 1 1 calc R . .
H9C H 0.1455 0.3786 0.0566 0.063 Uiso 1 1 calc R . .
C10 C -0.0314(8) 0.6253(6) 0.4470(5) 0.0362(18) Uani 1 1 d . . .
H10A H -0.0584 0.6963 0.4440 0.054 Uiso 1 1 calc R . .
H10B H 0.0379 0.6196 0.4844 0.054 Uiso 1 1 calc R . .
H10C H -0.1005 0.5830 0.4654 0.054 Uiso 1 1 calc R . .
Cl1 Cl 0.2500 0.7500 0.39815(14) 0.0343(6) Uani 1 2 d S . .
Cl2 Cl 0.13827(16) 0.82774(12) 0.23523(11) 0.0273(4) Uani 1 1 d . . .
Ru1 Ru 0.15240(5) 0.65540(4) 0.29000(3) 0.02361(18) Uani 1 1 d . . .
B1 B 0.768(2) 0.757(2) 0.1155(8) 0.031(4) Uiso 0.50 1 d P A -1
F1 F 0.8933(10) 0.7838(7) 0.1083(6) 0.047(2) Uani 0.50 1 d P A -1
F2 F 0.768(2) 0.755(4) 0.1977(4) 0.027(4) Uani 0.50 1 d P A -1
F3 F 0.699(2) 0.832(2) 0.0840(18) 0.058(7) Uani 0.50 1 d P A -1
F4 F 0.756(2) 0.6643(16) 0.0777(17) 0.054(6) Uani 0.50 1 d P A -1
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
C1 C6 1.404(11) . ?
C1 C2 1.428(10) . ?
C1 C7 1.516(10) . ?
C1 Ru1 2.167(7) . ?
C2 C3 1.393(10) . ?
C2 Ru1 2.165(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.422(10) . ?
C3 Ru1 2.157(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(10) . ?
C4 C10 1.518(10) . ?
C4 Ru1 2.171(7) . ?
C5 C6 1.424(10) . ?
C5 Ru1 2.156(7) . ?
C5 H5 0.9500 . ?
C6 Ru1 2.144(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.515(11) . ?
C7 C9 1.536(10) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
Cl1 Ru1 2.4438(19) . ?
Cl1 Ru1 2.4438(19) 2_565 ?
Cl2 Ru1 2.4481(18) 2_565 ?
Cl2 Ru1 2.4541(17) . ?
Ru1 Cl2 2.4481(18) 2_565 ?
B1 F3 1.35(4) . ?
B1 F4 1.38(3) . ?
B1 F2 1.384(15) . ?
B1 F1 1.40(2) . ?
 
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
C6 C1 C2 117.7(7) . . ?
C6 C1 C7 123.1(7) . . ?
C2 C1 C7 119.2(7) . . ?
C6 C1 Ru1 70.1(4) . . ?
C2 C1 Ru1 70.7(4) . . ?
C7 C1 Ru1 128.4(5) . . ?
C3 C2 C1 121.6(7) . . ?
C3 C2 Ru1 70.9(4) . . ?
C1 C2 Ru1 70.8(4) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
Ru1 C2 H2 132.2 . . ?
C2 C3 C4 120.8(7) . . ?
C2 C3 Ru1 71.5(4) . . ?
C4 C3 Ru1 71.4(4) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
Ru1 C3 H3 130.2 . . ?
C5 C4 C3 118.2(7) . . ?
C5 C4 C10 121.3(7) . . ?
C3 C4 C10 120.4(7) . . ?
C5 C4 Ru1 70.4(4) . . ?
C3 C4 Ru1 70.3(4) . . ?
C10 C4 Ru1 127.9(5) . . ?
C4 C5 C6 120.8(7) . . ?
C4 C5 Ru1 71.6(4) . . ?
C6 C5 Ru1 70.2(4) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
Ru1 C5 H5 131.5 . . ?
C1 C6 C5 120.9(7) . . ?
C1 C6 Ru1 71.9(4) . . ?
C5 C6 Ru1 71.1(4) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
Ru1 C6 H6 130.1 . . ?
C8 C7 C1 114.4(6) . . ?
C8 C7 C9 111.3(7) . . ?
C1 C7 C9 109.2(6) . . ?
C8 C7 H7 107.2 . . ?
C1 C7 H7 107.2 . . ?
C9 C7 H7 107.2 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Ru1 Cl1 Ru1 83.72(8) . 2_565 ?
Ru1 Cl2 Ru1 83.41(6) 2_565 . ?
C6 Ru1 C5 38.7(3) . . ?
C6 Ru1 C3 81.6(3) . . ?
C5 Ru1 C3 68.6(3) . . ?
C6 Ru1 C2 68.5(3) . . ?
C5 Ru1 C2 80.8(3) . . ?
C3 Ru1 C2 37.6(3) . . ?
C6 Ru1 C1 38.0(3) . . ?
C5 Ru1 C1 69.4(3) . . ?
C3 Ru1 C1 69.4(3) . . ?
C2 Ru1 C1 38.5(3) . . ?
C6 Ru1 C4 69.7(3) . . ?
C5 Ru1 C4 38.1(3) . . ?
C3 Ru1 C4 38.4(3) . . ?
C2 Ru1 C4 68.7(3) . . ?
C1 Ru1 C4 82.8(3) . . ?
C6 Ru1 Cl1 155.8(2) . . ?
C5 Ru1 Cl1 118.4(2) . . ?
C3 Ru1 Cl1 96.8(2) . . ?
C2 Ru1 Cl1 123.5(2) . . ?
C1 Ru1 Cl1 161.4(2) . . ?
C4 Ru1 Cl1 94.1(2) . . ?
C6 Ru1 Cl2 121.5(2) . 2_565 ?
C5 Ru1 Cl2 160.0(2) . 2_565 ?
C3 Ru1 Cl2 117.8(2) . 2_565 ?
C2 Ru1 Cl2 93.9(2) . 2_565 ?
C1 Ru1 Cl2 94.5(2) . 2_565 ?
C4 Ru1 Cl2 155.3(2) . 2_565 ?
Cl1 Ru1 Cl2 80.63(5) . 2_565 ?
C6 Ru1 Cl2 93.1(2) . . ?
C5 Ru1 Cl2 96.06(19) . . ?
C3 Ru1 Cl2 161.2(2) . . ?
C2 Ru1 Cl2 154.4(2) . . ?
C1 Ru1 Cl2 116.59(19) . . ?
C4 Ru1 Cl2 122.9(2) . . ?
Cl1 Ru1 Cl2 80.51(5) . . ?
Cl2 Ru1 Cl2 80.33(7) 2_565 . ?
F3 B1 F4 114.4(16) . . ?
F3 B1 F2 114(3) . . ?
F4 B1 F2 117(3) . . ?
F3 B1 F1 108.1(19) . . ?
F4 B1 F1 106.2(19) . . ?
F2 B1 F1 95.4(15) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    1.082
_refine_diff_density_min   -1.570
_refine_diff_density_rms    0.178
