#------------------------------------------------------------------------------
#$Date: 2017-10-14 21:27:35 +0200 (Sat 14 de Oct de 2017) $
#$Revision: 202017 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/05/7050521.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_7050521
loop_
_publ_author_name
'Laye, Rebecca H.'
'Bell, Zöe R.'
'Ward, Michael D.'
_publ_section_title
;
 Complexes of 2,2'-biphenol with ruthenium(ii), molybdenum(v),
 tungsten(v) and tungsten(vi): structures, electrochemistry and
 spectroscopy
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              684
_journal_paper_doi               10.1039/b211997h
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C36 H24 Cl6 O6 W2'
_chemical_formula_weight         1132.95
_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                90.00
_cell_angle_beta                 93.85(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.985(2)
_cell_length_b                   22.734(5)
_cell_length_c                   16.038(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3632.4(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens SMART Area Detector'
_diffrn_measurement_method
'ω rotation with narrow frames (0.3 degrees)'
_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  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23703
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    6.816
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0224P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                5235
_reflns_number_total             8307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211997h.txt
_cod_data_source_block           freshs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3632.2(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7050521
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
W1 W 0.72008(3) -0.379167(12) 0.580634(18) 0.02001(8) Uani 1 1 d . . .
W2 W 0.54881(3) -0.161103(12) 0.630517(18) 0.02096(8) Uani 1 1 d . . .
Cl11 Cl 0.51410(18) -0.34318(8) 0.52807(12) 0.0302(4) Uani 1 1 d . . .
Cl12 Cl 0.93117(18) -0.41400(8) 0.63076(11) 0.0295(4) Uani 1 1 d . . .
Cl13 Cl 0.80654(19) -0.34223(8) 0.45918(11) 0.0290(4) Uani 1 1 d . . .
Cl21 Cl 0.35215(19) -0.20182(9) 0.56879(13) 0.0380(5) Uani 1 1 d . . .
Cl22 Cl 0.6591(2) -0.19609(8) 0.51692(11) 0.0340(5) Uani 1 1 d . . .
Cl23 Cl 0.4287(2) -0.12627(8) 0.74047(12) 0.0366(5) Uani 1 1 d . . .
O11 O 0.6249(5) -0.40991(19) 0.6678(3) 0.0234(11) Uani 1 1 d . . .
O12 O 0.7004(5) -0.45293(19) 0.5321(3) 0.0213(11) Uani 1 1 d . . .
O13 O 0.7651(5) -0.31286(19) 0.6436(3) 0.0238(11) Uani 1 1 d . . .
O21 O 0.7122(5) -0.1274(2) 0.6696(3) 0.0305(12) Uani 1 1 d . . .
O22 O 0.5102(5) -0.0886(2) 0.5790(3) 0.0241(11) Uani 1 1 d . . .
O23 O 0.5845(5) -0.22700(19) 0.6956(3) 0.0243(11) Uani 1 1 d . . .
C111 C 0.5159(7) -0.4467(3) 0.6711(4) 0.0243(17) Uani 1 1 d . . .
C112 C 0.5205(7) -0.5058(3) 0.6462(4) 0.0253(17) Uani 1 1 d . . .
C113 C 0.4051(8) -0.5384(3) 0.6525(4) 0.033(2) Uani 1 1 d . . .
H11A H 0.4053 -0.5788 0.6373 0.040 Uiso 1 1 calc R . .
C114 C 0.2895(8) -0.5142(4) 0.6801(5) 0.040(2) Uani 1 1 d . . .
H11B H 0.2111 -0.5376 0.6829 0.048 Uiso 1 1 calc R . .
C115 C 0.2880(8) -0.4554(4) 0.7038(5) 0.041(2) Uani 1 1 d . . .
H11C H 0.2079 -0.4382 0.7213 0.049 Uiso 1 1 calc R . .
C116 C 0.4030(7) -0.4221(4) 0.7019(4) 0.0324(19) Uani 1 1 d . . .
H11D H 0.4045 -0.3827 0.7216 0.039 Uiso 1 1 calc R . .
C121 C 0.7237(7) -0.5110(3) 0.5558(4) 0.0255(17) Uani 1 1 d . . .
C122 C 0.6415(7) -0.5354(3) 0.6138(4) 0.0233(16) Uani 1 1 d . . .
C123 C 0.6717(8) -0.5934(3) 0.6377(4) 0.0306(18) Uani 1 1 d . . .
H12A H 0.6184 -0.6124 0.6765 0.037 Uiso 1 1 calc R . .
C124 C 0.7785(8) -0.6238(3) 0.6058(5) 0.0354(19) Uani 1 1 d . . .
H12B H 0.8003 -0.6625 0.6248 0.043 Uiso 1 1 calc R . .
C125 C 0.8527(8) -0.5970(3) 0.5459(5) 0.037(2) Uani 1 1 d . . .
H12C H 0.9223 -0.6184 0.5221 0.044 Uiso 1 1 calc R . .
C126 C 0.8267(7) -0.5399(3) 0.5208(4) 0.0266(18) Uani 1 1 d . . .
H12D H 0.8782 -0.5213 0.4806 0.032 Uiso 1 1 calc R . .
C131 C 0.8604(7) -0.2839(3) 0.6947(4) 0.0243(17) Uani 1 1 d . . .
C132 C 0.8278(7) -0.2704(3) 0.7759(4) 0.0247(17) Uani 1 1 d . . .
C133 C 0.9318(8) -0.2459(3) 0.8287(5) 0.0319(19) Uani 1 1 d . . .
H13A H 0.9168 -0.2380 0.8854 0.038 Uiso 1 1 calc R . .
C134 C 1.0544(8) -0.2334(3) 0.7994(6) 0.038(2) Uani 1 1 d . . .
H13B H 1.1224 -0.2159 0.8355 0.046 Uiso 1 1 calc R . .
C135 C 1.0801(8) -0.2461(3) 0.7170(6) 0.039(2) Uani 1 1 d . . .
H13C H 1.1646 -0.2368 0.6965 0.047 Uiso 1 1 calc R . .
C136 C 0.9816(7) -0.2723(3) 0.6657(5) 0.0319(19) Uani 1 1 d . . .
H13D H 0.9987 -0.2822 0.6099 0.038 Uiso 1 1 calc R . .
C211 C 0.8008(7) -0.0865(3) 0.6479(4) 0.0263(17) Uani 1 1 d . . .
C212 C 0.7649(7) -0.0277(3) 0.6297(4) 0.0251(17) Uani 1 1 d . . .
C213 C 0.8700(8) 0.0091(3) 0.6097(5) 0.0333(19) Uani 1 1 d . . .
H21A H 0.8501 0.0488 0.5953 0.040 Uiso 1 1 calc R . .
C214 C 0.9997(8) -0.0094(4) 0.6100(5) 0.041(2) Uani 1 1 d . . .
H21B H 1.0678 0.0174 0.5965 0.049 Uiso 1 1 calc R . .
C215 C 1.0332(8) -0.0674(3) 0.6299(5) 0.036(2) Uani 1 1 d . . .
H21C H 1.1237 -0.0804 0.6307 0.043 Uiso 1 1 calc R . .
C216 C 0.9331(8) -0.1051(3) 0.6483(5) 0.035(2) Uani 1 1 d . . .
H21D H 0.9544 -0.1448 0.6617 0.042 Uiso 1 1 calc R . .
C221 C 0.5073(7) -0.0307(3) 0.5996(4) 0.0241(17) Uani 1 1 d . . .
C222 C 0.6268(8) -0.0020(3) 0.6291(4) 0.0253(17) Uani 1 1 d . . .
C223 C 0.6129(8) 0.0572(3) 0.6531(5) 0.034(2) Uani 1 1 d . . .
H22A H 0.6885 0.0780 0.6771 0.040 Uiso 1 1 calc R . .
C224 C 0.4904(9) 0.0853(3) 0.6421(5) 0.035(2) Uani 1 1 d . . .
H22B H 0.4836 0.1253 0.6581 0.042 Uiso 1 1 calc R . .
C225 C 0.3779(8) 0.0566(3) 0.6084(5) 0.0317(19) Uani 1 1 d . . .
H22C H 0.2954 0.0770 0.5985 0.038 Uiso 1 1 calc R . .
C226 C 0.3873(7) -0.0017(3) 0.5895(4) 0.0244(17) Uani 1 1 d . . .
H22D H 0.3094 -0.0225 0.5690 0.029 Uiso 1 1 calc R . .
C231 C 0.5765(7) -0.2607(3) 0.7657(4) 0.0225(17) Uani 1 1 d . . .
C232 C 0.6936(8) -0.2822(3) 0.8066(4) 0.0230(17) Uani 1 1 d . . .
C233 C 0.6796(9) -0.3134(3) 0.8805(5) 0.035(2) Uani 1 1 d . . .
H23A H 0.7569 -0.3291 0.9103 0.042 Uiso 1 1 calc R . .
C234 C 0.5537(10) -0.3218(4) 0.9111(5) 0.049(3) Uani 1 1 d . . .
H23B H 0.5464 -0.3430 0.9616 0.059 Uiso 1 1 calc R . .
C235 C 0.4424(10) -0.3003(3) 0.8700(5) 0.042(2) Uani 1 1 d . . .
H23C H 0.3573 -0.3067 0.8916 0.051 Uiso 1 1 calc R . .
C236 C 0.4514(8) -0.2688(3) 0.7960(5) 0.0312(19) Uani 1 1 d . . .
H23D H 0.3732 -0.2533 0.7671 0.037 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'
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'
W W -0.8490 6.8722 '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
O13 W1 O12 168.5(2) . . ?
O13 W1 O11 90.76(19) . . ?
O12 W1 O11 86.05(18) . . ?
O13 W1 Cl11 95.05(15) . . ?
O12 W1 Cl11 95.75(15) . . ?
O11 W1 Cl11 85.47(15) . . ?
O13 W1 Cl13 94.15(14) . . ?
O12 W1 Cl13 90.57(14) . . ?
O11 W1 Cl13 170.91(15) . . ?
Cl11 W1 Cl13 86.47(7) . . ?
O13 W1 Cl12 84.73(15) . . ?
O12 W1 Cl12 84.60(15) . . ?
O11 W1 Cl12 96.17(15) . . ?
Cl11 W1 Cl12 178.35(7) . . ?
Cl13 W1 Cl12 91.91(7) . . ?
O23 W2 O22 171.78(19) . . ?
O23 W2 O21 90.7(2) . . ?
O22 W2 O21 86.4(2) . . ?
O23 W2 Cl21 92.46(16) . . ?
O22 W2 Cl21 91.11(15) . . ?
O21 W2 Cl21 174.42(15) . . ?
O23 W2 Cl22 94.68(14) . . ?
O22 W2 Cl22 92.86(14) . . ?
O21 W2 Cl22 87.39(16) . . ?
Cl21 W2 Cl22 87.77(7) . . ?
O23 W2 Cl23 86.43(14) . . ?
O22 W2 Cl23 86.18(14) . . ?
O21 W2 Cl23 95.09(16) . . ?
Cl21 W2 Cl23 89.69(8) . . ?
Cl22 W2 Cl23 177.27(8) . . ?
C111 O11 W1 134.0(4) . . ?
C121 O12 W1 137.2(4) . . ?
C131 O13 W1 147.6(4) . . ?
C211 O21 W2 140.4(4) . . ?
C221 O22 W2 138.9(4) . . ?
C231 O23 W2 154.1(4) . . ?
O11 C111 C116 115.8(6) . . ?
O11 C111 C112 122.0(6) . . ?
C116 C111 C112 122.2(7) . . ?
C113 C112 C111 116.8(7) . . ?
C113 C112 C122 118.5(7) . . ?
C111 C112 C122 124.7(6) . . ?
C114 C113 C112 122.0(7) . . ?
C113 C114 C115 119.7(7) . . ?
C116 C115 C114 119.9(8) . . ?
C115 C116 C111 119.2(7) . . ?
C126 C121 O12 117.4(6) . . ?
C126 C121 C122 124.9(7) . . ?
O12 C121 C122 117.7(6) . . ?
C121 C122 C123 115.6(6) . . ?
C121 C122 C112 125.0(6) . . ?
C123 C122 C112 119.3(6) . . ?
C124 C123 C122 121.4(7) . . ?
C125 C124 C123 119.4(7) . . ?
C126 C125 C124 121.0(7) . . ?
C121 C126 C125 117.6(7) . . ?
C136 C131 O13 119.1(6) . . ?
C136 C131 C132 123.2(7) . . ?
O13 C131 C132 117.6(6) . . ?
C131 C132 C133 116.0(7) . . ?
C131 C132 C232 122.8(7) . . ?
C133 C132 C232 121.2(6) . . ?
C134 C133 C132 121.1(7) . . ?
C133 C134 C135 120.5(8) . . ?
C136 C135 C134 119.2(8) . . ?
C131 C136 C135 120.0(7) . . ?
O21 C211 C216 115.5(7) . . ?
O21 C211 C212 123.2(7) . . ?
C216 C211 C212 121.2(7) . . ?
C213 C212 C211 115.6(7) . . ?
C213 C212 C222 118.1(6) . . ?
C211 C212 C222 126.3(7) . . ?
C214 C213 C212 122.9(8) . . ?
C213 C214 C215 120.5(8) . . ?
C216 C215 C214 118.4(7) . . ?
C215 C216 C211 121.3(7) . . ?
O22 C221 C226 118.1(7) . . ?
O22 C221 C222 119.8(6) . . ?
C226 C221 C222 122.1(7) . . ?
C223 C222 C221 115.8(7) . . ?
C223 C222 C212 118.5(7) . . ?
C221 C222 C212 125.5(6) . . ?
C224 C223 C222 120.6(7) . . ?
C225 C224 C223 121.5(7) . . ?
C226 C225 C224 118.8(7) . . ?
C225 C226 C221 120.9(7) . . ?
O23 C231 C236 117.9(7) . . ?
O23 C231 C232 119.4(6) . . ?
C236 C231 C232 122.5(6) . . ?
C231 C232 C233 116.7(7) . . ?
C231 C232 C132 122.0(6) . . ?
C233 C232 C132 121.2(7) . . ?
C234 C233 C232 120.9(8) . . ?
C235 C234 C233 120.9(8) . . ?
C234 C235 C236 120.3(8) . . ?
C231 C236 C235 118.6(8) . . ?
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
W1 O13 1.853(4) . ?
W1 O12 1.854(4) . ?
W1 O11 1.878(4) . ?
W1 Cl11 2.3189(19) . ?
W1 Cl13 2.3388(17) . ?
W1 Cl12 2.3426(19) . ?
W2 O23 1.847(4) . ?
W2 O22 1.871(5) . ?
W2 O21 1.872(5) . ?
W2 Cl21 2.331(2) . ?
W2 Cl22 2.3308(18) . ?
W2 Cl23 2.3366(18) . ?
O11 C111 1.375(8) . ?
O12 C121 1.389(8) . ?
O13 C131 1.380(8) . ?
O21 C211 1.345(8) . ?
O22 C221 1.359(8) . ?
O23 C231 1.367(7) . ?
C111 C116 1.380(9) . ?
C111 C112 1.403(9) . ?
C112 C113 1.380(9) . ?
C112 C122 1.507(10) . ?
C113 C114 1.379(10) . ?
C114 C115 1.390(11) . ?
C115 C116 1.377(10) . ?
C121 C126 1.372(9) . ?
C121 C122 1.396(9) . ?
C122 C123 1.401(9) . ?
C123 C124 1.396(10) . ?
C124 C125 1.392(10) . ?
C125 C126 1.379(10) . ?
C131 C136 1.351(9) . ?
C131 C132 1.398(9) . ?
C132 C133 1.409(10) . ?
C132 C232 1.482(10) . ?
C133 C134 1.370(10) . ?
C134 C135 1.392(11) . ?
C135 C136 1.375(10) . ?
C211 C216 1.386(10) . ?
C211 C212 1.409(9) . ?
C212 C213 1.395(10) . ?
C212 C222 1.497(10) . ?
C213 C214 1.362(11) . ?
C214 C215 1.392(11) . ?
C215 C216 1.364(10) . ?
C221 C226 1.367(9) . ?
C221 C222 1.412(10) . ?
C222 C223 1.410(9) . ?
C223 C224 1.380(10) . ?
C224 C225 1.378(10) . ?
C225 C226 1.364(9) . ?
C231 C236 1.383(9) . ?
C231 C232 1.391(10) . ?
C232 C233 1.396(9) . ?
C233 C234 1.393(11) . ?
C234 C235 1.345(12) . ?
C235 C236 1.394(10) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652842
