#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/75/7027581.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027581
loop_
_publ_author_name
'Zhou, Xiang-Ge'
'Huang, Jie-Sheng'
'Ko, Po-Hung'
'Cheung, Kung-Kai'
'Che, Chi-Ming'
_publ_contact_author
;
    ENTER NAME
 ENTER ADDRESS
;
_publ_section_title
;
 Titanium and ruthenium binaphthyl Schiff base complexes as catalysts for
 asymmetric trimethylsilylcyanation of aldehydes
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3303
_journal_paper_doi               10.1039/a904330f
_journal_year                    1999
_chemical_formula_moiety         'C34 H16 Cl5 N3 O3 Ru . CH2Cl2'
_chemical_formula_sum            'C35 H20 Cl7 N3 O3 Ru'
_chemical_formula_weight         879.80
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Wed Apr 21 10:36:09 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                81.70(3)
_cell_angle_beta                 72.34(3)
_cell_angle_gamma                83.89(3)
_cell_formula_units_Z            2
_cell_length_a                   11.555(5)
_cell_length_b                   12.087(4)
_cell_length_c                   13.347(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      21.5
_cell_volume                     1753.8(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      298.2
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.03913
_diffrn_orient_matrix_UB_12      -0.07653
_diffrn_orient_matrix_UB_13      -0.01300
_diffrn_orient_matrix_UB_21      0.07902
_diffrn_orient_matrix_UB_22      0.02479
_diffrn_orient_matrix_UB_23      0.00203
_diffrn_orient_matrix_UB_31      0.02257
_diffrn_orient_matrix_UB_32      0.02344
_diffrn_orient_matrix_UB_33      -0.07809
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  4.23
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4840
_diffrn_reflns_theta_max         22.51
_diffrn_standards_decay_%        -2.83
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       prism
_exptl_crystal_F_000             876.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.81
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.845
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         3085
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0397
_refine_ls_shift/esd_max         1.5350
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0498
_reflns_number_observed          3085
_reflns_number_total             4574
_reflns_observed_criterion       3.00
_cod_data_source_file            904330Fsup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        1753(2)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C35 H20 Cl7 N3 O3 Ru '
_cod_database_code               7027581
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Ru(1) 0.13797(6) 0.44878(5) 0.71317(5) 0.0320 Uij
Cl(1) 0.0816(2) 0.3410(2) 0.6031(2) 0.0476 Uij
Cl(2) -0.2275(2) 0.2955(2) 0.9204(2) 0.0538 Uij
Cl(3) -0.4879(2) 0.5694(2) 0.7045(2) 0.0673 Uij
Cl(4) 0.2839(2) 0.0785(2) 0.8336(2) 0.0614 Uij
Cl(5) 0.4718(2) 0.2474(2) 1.0968(2) 0.0765 Uij
Cl(6) -0.3472(5) 1.0434(4) 0.7785(4) 0.1752 Uij
Cl(7) -0.1895(4) 0.9268(5) 0.6050(4) 0.1718 Uij
O(1) 0.3784(5) 0.4476(5) 0.5655(5) 0.0615 Uij
O(2) -0.0302(4) 0.4391(4) 0.8076(4) 0.0387 Uij
O(3) 0.1836(5) 0.3047(4) 0.7970(4) 0.0420 Uij
N(1) 0.2837(6) 0.4509(5) 0.6277(5) 0.0377 Uij
N(2) 0.0753(5) 0.5903(4) 0.6360(4) 0.0306 Uij
N(3) 0.1684(5) 0.5446(5) 0.8187(4) 0.0335 Uij
C(1) -0.1289(7) 0.4684(6) 0.7773(6) 0.0353 Uij
C(2) -0.2340(7) 0.4107(6) 0.8273(6) 0.0395 Uij
C(3) -0.3430(7) 0.4401(7) 0.8060(6) 0.0432 Uij
C(4) -0.3509(7) 0.5307(7) 0.7316(6) 0.0436 Uij
C(5) -0.2494(7) 0.5890(6) 0.6790(6) 0.0445 Uij
C(6) -0.1380(6) 0.5576(6) 0.6999(6) 0.0348 Uij
C(7) -0.0341(7) 0.6209(6) 0.6383(6) 0.0372 Uij
C(8) 0.1737(6) 0.6620(6) 0.5780(5) 0.0321 Uij
C(9) 0.2287(7) 0.6537(6) 0.4701(6) 0.0456 Uij
C(10) 0.3369(8) 0.7020(6) 0.4211(6) 0.0524 Uij
C(11) 0.3920(7) 0.7589(6) 0.4776(6) 0.0448 Uij
C(12) 0.5074(8) 0.8015(7) 0.4299(7) 0.0655 Uij
C(13) 0.5605(8) 0.8554(8) 0.4859(9) 0.0730 Uij
C(14) 0.5023(8) 0.8683(7) 0.5912(9) 0.0667 Uij
C(15) 0.3905(7) 0.8282(6) 0.6409(6) 0.0472 Uij
C(16) 0.3321(7) 0.7708(6) 0.5856(6) 0.0353 Uij
C(17) 0.2193(6) 0.7222(5) 0.6353(5) 0.0311 Uij
C(18) 0.1428(6) 0.7418(6) 0.7441(6) 0.0349 Uij
C(19) 0.0906(6) 0.8522(6) 0.7604(6) 0.0333 Uij
C(20) 0.1104(7) 0.9428(6) 0.6775(6) 0.0456 Uij
C(21) 0.0641(8) 1.0483(6) 0.6954(7) 0.0547 Uij
C(22) -0.0056(9) 1.0719(7) 0.7958(8) 0.0620 Uij
C(23) -0.0302(8) 0.9886(7) 0.8768(7) 0.0539 Uij
C(24) 0.0185(6) 0.8769(6) 0.8615(6) 0.0371 Uij
C(25) -0.0046(7) 0.7886(7) 0.9451(6) 0.0456 Uij
C(26) 0.0415(7) 0.6827(6) 0.9299(6) 0.0421 Uij
C(27) 0.1176(6) 0.6587(6) 0.8289(5) 0.0307 Uij
C(28) 0.2262(7) 0.5022(6) 0.8865(6) 0.0396 Uij
C(29) 0.2743(7) 0.3903(6) 0.9053(6) 0.0398 Uij
C(30) 0.3430(7) 0.3708(7) 0.9783(6) 0.0461 Uij
C(31) 0.3897(7) 0.2671(7) 1.0048(6) 0.0477 Uij
C(32) 0.3734(8) 0.1778(7) 0.9586(6) 0.0498 Uij
C(33) 0.3067(7) 0.1915(6) 0.8878(6) 0.0412 Uij
C(34) 0.2525(7) 0.2977(6) 0.8584(6) 0.0365 Uij
C(35) -0.230(1) 0.932(2) 0.725(1) 0.2109 Uij
H(1) -0.4123 0.3986 0.8417 0.0510 Uij
H(2) -0.2551 0.6510 0.6281 0.0531 Uij
H(3) -0.0494 0.6893 0.5978 0.0439 Uij
H(4) 0.1915 0.6156 0.4316 0.0540 Uij
H(5) 0.3757 0.6963 0.3481 0.0627 Uij
H(6) 0.5489 0.7926 0.3580 0.0774 Uij
H(7) 0.6380 0.8843 0.4522 0.0868 Uij
H(8) 0.5410 0.9056 0.6293 0.0794 Uij
H(9) 0.3511 0.8388 0.7130 0.0562 Uij
H(10) 0.1570 0.9291 0.6077 0.0539 Uij
H(11) 0.0796 1.1070 0.6385 0.0642 Uij
H(12) -0.0353 1.1466 0.8073 0.0738 Uij
H(13) -0.0807 1.0045 0.9447 0.0637 Uij
H(14) -0.0537 0.8037 1.0136 0.0537 Uij
H(15) 0.0231 0.6240 0.9869 0.0490 Uij
H(16) 0.2378 0.5531 0.9300 0.0468 Uij
H(17) 0.3569 0.4321 1.0096 0.0550 Uij
H(18) 0.4082 0.1057 0.9763 0.0586 Uij
H(19) -0.1620 0.9260 0.7516 0.1940 Uij
H(20) -0.2679 0.8539 0.7579 0.1940 Uij
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ru 0 2 -1.259 0.836 'International Tables'
Cl 0 14 0.148 0.159 'International Tables'
O 0 6 0.011 0.006 'International Tables'
N 0 6 0.006 0.003 'International Tables'
C 0 70 0.003 0.002 'International Tables'
H 0 40 0.000 0.000 'International Tables'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cl(1) Ru(1) O(2) 87.0(2) yes
Cl(1) Ru(1) O(3) 89.6(1) yes
Cl(1) Ru(1) N(1) 90.0(2) yes
Cl(1) Ru(1) N(2) 88.9(2) yes
Cl(1) Ru(1) N(3) 174.0(2) yes
O(2) Ru(1) O(3) 87.9(2) yes
O(2) Ru(1) N(1) 176.8(3) yes
O(2) Ru(1) N(2) 86.8(2) yes
O(2) Ru(1) N(3) 87.1(2) yes
O(3) Ru(1) N(1) 91.0(2) yes
O(3) Ru(1) N(2) 174.6(2) yes
O(3) Ru(1) N(3) 91.1(2) yes
N(1) Ru(1) N(2) 94.2(2) yes
N(1) Ru(1) N(3) 95.9(3) yes
N(2) Ru(1) N(3) 89.9(2) yes
Ru(1) O(2) C(1) 124.6(4) yes
Ru(1) O(3) C(34) 125.0(4) yes
Ru(1) N(1) O(1) 174.7(6) yes
Ru(1) N(2) C(7) 127.9(5) yes
Ru(1) N(2) C(8) 111.5(4) yes
C(7) N(2) C(8) 120.5(6) yes
Ru(1) N(3) C(27) 122.8(4) yes
Ru(1) N(3) C(28) 121.5(5) yes
C(27) N(3) C(28) 115.4(6) yes
O(2) C(1) C(2) 119.2(7) yes
O(2) C(1) C(6) 124.2(6) yes
C(2) C(1) C(6) 116.6(7) yes
Cl(2) C(2) C(1) 119.0(6) yes
Cl(2) C(2) C(3) 117.8(6) yes
C(1) C(2) C(3) 123.2(7) yes
C(2) C(3) C(4) 119.2(7) yes
Cl(3) C(4) C(3) 119.8(6) yes
Cl(3) C(4) C(5) 120.5(6) yes
C(3) C(4) C(5) 119.7(7) yes
C(4) C(5) C(6) 120.8(7) yes
C(1) C(6) C(5) 120.4(7) yes
C(1) C(6) C(7) 122.2(6) yes
C(5) C(6) C(7) 117.5(7) yes
N(2) C(7) C(6) 123.8(6) yes
N(2) C(8) C(9) 118.7(6) yes
N(2) C(8) C(17) 117.7(6) yes
C(9) C(8) C(17) 122.8(7) yes
C(8) C(9) C(10) 118.6(7) yes
C(9) C(10) C(11) 121.0(7) yes
C(10) C(11) C(12) 121.3(8) yes
C(10) C(11) C(16) 119.5(7) yes
C(12) C(11) C(16) 119.1(8) yes
C(11) C(12) C(13) 120.8(8) yes
C(12) C(13) C(14) 120.5(8) yes
C(13) C(14) C(15) 120.8(9) yes
C(14) C(15) C(16) 120.5(8) yes
C(11) C(16) C(15) 118.2(7) yes
C(11) C(16) C(17) 119.1(7) yes
C(15) C(16) C(17) 122.6(7) yes
C(8) C(17) C(16) 118.7(6) yes
C(8) C(17) C(18) 118.3(6) yes
C(16) C(17) C(18) 122.8(6) yes
C(17) C(18) C(19) 117.8(6) yes
C(17) C(18) C(27) 123.9(6) yes
C(19) C(18) C(27) 118.4(7) yes
C(18) C(19) C(20) 122.3(7) yes
C(18) C(19) C(24) 120.8(6) yes
C(20) C(19) C(24) 116.9(6) yes
C(19) C(20) C(21) 121.5(7) yes
C(20) C(21) C(22) 121.0(8) yes
C(21) C(22) C(23) 120.0(7) yes
C(22) C(23) C(24) 120.6(8) yes
C(19) C(24) C(23) 119.9(7) yes
C(19) C(24) C(25) 118.4(7) yes
C(23) C(24) C(25) 121.8(7) yes
C(24) C(25) C(26) 121.4(7) yes
C(25) C(26) C(27) 120.1(7) yes
N(3) C(27) C(18) 121.6(6) yes
N(3) C(27) C(26) 117.5(6) yes
C(18) C(27) C(26) 120.9(7) yes
N(3) C(28) C(29) 129.3(7) yes
C(28) C(29) C(30) 116.6(7) yes
C(28) C(29) C(34) 124.0(7) yes
C(30) C(29) C(34) 119.3(7) yes
C(29) C(30) C(31) 121.7(8) yes
Cl(5) C(31) C(30) 119.8(7) yes
Cl(5) C(31) C(32) 120.1(6) yes
C(30) C(31) C(32) 120.1(7) yes
C(31) C(32) C(33) 120.8(7) yes
Cl(4) C(33) C(32) 120.2(6) yes
Cl(4) C(33) C(34) 117.7(6) yes
C(32) C(33) C(34) 122.1(7) yes
O(3) C(34) C(29) 124.3(7) yes
O(3) C(34) C(33) 119.6(7) yes
C(29) C(34) C(33) 116.0(7) yes
Cl(6) C(35) Cl(7) 118(1) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ru(1) Cl(1) 2.365(2) yes
Ru(1) O(2) 1.974(5) yes
Ru(1) O(3) 2.040(5) yes
Ru(1) N(1) 1.724(7) yes
Ru(1) N(2) 2.046(6) yes
Ru(1) N(3) 2.075(6) yes
Cl(2) C(2) 1.739(8) yes
Cl(3) C(4) 1.731(8) yes
Cl(4) C(33) 1.715(8) yes
Cl(5) C(31) 1.743(8) yes
Cl(6) C(35) 1.86(2) yes
Cl(7) C(35) 1.53(2) yes
O(1) N(1) 1.157(7) yes
O(2) C(1) 1.319(8) yes
O(3) C(34) 1.295(8) yes
N(2) C(7) 1.271(9) yes
N(2) C(8) 1.458(8) yes
N(3) C(27) 1.449(9) yes
N(3) C(28) 1.299(9) yes
C(1) C(2) 1.400(10) yes
C(1) C(6) 1.401(10) yes
C(2) C(3) 1.37(1) yes
C(3) C(4) 1.38(1) yes
C(4) C(5) 1.38(1) yes
C(5) C(6) 1.40(1) yes
C(6) C(7) 1.455(10) yes
C(8) C(9) 1.400(10) yes
C(8) C(17) 1.370(9) yes
C(9) C(10) 1.37(1) yes
C(10) C(11) 1.41(1) yes
C(11) C(12) 1.41(1) yes
C(11) C(16) 1.42(1) yes
C(12) C(13) 1.37(1) yes
C(13) C(14) 1.39(1) yes
C(14) C(15) 1.37(1) yes
C(15) C(16) 1.42(1) yes
C(16) C(17) 1.418(9) yes
C(17) C(18) 1.491(9) yes
C(18) C(19) 1.423(9) yes
C(18) C(27) 1.381(9) yes
C(19) C(20) 1.424(10) yes
C(19) C(24) 1.409(10) yes
C(20) C(21) 1.35(1) yes
C(21) C(22) 1.39(1) yes
C(22) C(23) 1.35(1) yes
C(23) C(24) 1.42(1) yes
C(24) C(25) 1.41(1) yes
C(25) C(26) 1.35(1) yes
C(26) C(27) 1.419(10) yes
C(28) C(29) 1.42(1) yes
C(29) C(30) 1.41(1) yes
C(29) C(34) 1.44(1) yes
C(30) C(31) 1.35(1) yes
C(31) C(32) 1.37(1) yes
C(32) C(33) 1.37(1) yes
C(33) C(34) 1.423(10) yes
