#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:03:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179090 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/52/4305227.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_4305227
loop_
_publ_author_name
'Stefan Tampier'
'Rainer Müller'
'Andrea Thorn'
'Eike Hübner'
'Nicolai Burzlaff'
_publ_contact_author             'Burzlaff, Nicolai'
_publ_contact_author_email       burzlaff@chemie.uni-erlangen.de
_publ_section_title
;
Synthesis, Structure, and Reactivity of Ruthenium Carboxylato and
2-Oxocarboxylato Complexes Bearing the Bis(3,5-dimethylpyrazol-1-yl)acetato
Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9624
_journal_page_last               9641
_journal_paper_doi               10.1021/ic8000224
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H33 Cl N5 O2 P Ru, 2 (C H2 Cl2)'
_chemical_formula_sum            'C34 H37 Cl5 N5 O2 P Ru'
_chemical_formula_weight         856.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-03-01T14:45:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 110.040(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.715(4)
_cell_length_b                   10.9196(11)
_cell_length_c                   20.288(4)
_cell_measurement_reflns_used    4
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      13.961
_cell_measurement_theta_min      11.371
_cell_measurement_wavelength     0.71073
_cell_volume                     3686.9(12)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.00377
_diffrn_orient_matrix_UB_12      0.05233
_diffrn_orient_matrix_UB_13      -0.04151
_diffrn_orient_matrix_UB_21      0.01608
_diffrn_orient_matrix_UB_22      0.073299
_diffrn_orient_matrix_UB_23      0.031333
_diffrn_orient_matrix_UB_31      0.057762
_diffrn_orient_matrix_UB_32      -0.016967
_diffrn_orient_matrix_UB_33      0.007307
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.059
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8269
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        -2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.87
_exptl_absorpt_correction_T_max  0.7703
_exptl_absorpt_correction_T_min  0.5158
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal columns'
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0483P)²+2.2192P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                5962
_reflns_number_total             8001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8000224-file002_1.cif
_cod_data_source_block           complex4
_cod_original_cell_volume        3686.8(11)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4305227
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
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 0.0940(2) 0.7712(3) 0.55692(17) 0.0234(7) Uani 1 1 d . . .
H1 H 0.1069 0.7713 0.5137 0.028 Uiso 1 1 calc R . .
C2 C 0.1544(2) 0.8545(3) 0.61017(17) 0.0217(7) Uani 1 1 d . . .
C11 C 0.0929(3) 0.4366(4) 0.7177(2) 0.0387(10) Uani 1 1 d . . .
H11A H 0.1448 0.4331 0.7537 0.058 Uiso 1 1 calc R . .
H11B H 0.0732 0.3549 0.7049 0.058 Uiso 1 1 calc R . .
H11C H 0.0563 0.4803 0.7349 0.058 Uiso 1 1 calc R . .
C12 C 0.0994(2) 0.5014(3) 0.65458(19) 0.0271(8) Uani 1 1 d . . .
C13 C 0.1109(2) 0.4479(3) 0.59580(19) 0.0297(8) Uani 1 1 d . . .
H13 H 0.1175 0.3649 0.589 0.036 Uiso 1 1 calc R . .
C14 C 0.1107(2) 0.5407(3) 0.55048(18) 0.0255(8) Uani 1 1 d . . .
C15 C 0.1174(2) 0.5373(4) 0.47865(19) 0.0353(9) Uani 1 1 d . . .
H15A H 0.07 0.5729 0.4453 0.053 Uiso 1 1 calc R . .
H15B H 0.1225 0.454 0.4658 0.053 Uiso 1 1 calc R . .
H15C H 0.1638 0.583 0.4789 0.053 Uiso 1 1 calc R . .
C21 C -0.1605(2) 0.8340(4) 0.5956(2) 0.0318(8) Uani 1 1 d . . .
H21A H -0.1794 0.7517 0.5963 0.048 Uiso 1 1 calc R . .
H21B H -0.2051 0.8861 0.5714 0.048 Uiso 1 1 calc R . .
H21C H -0.1356 0.8626 0.6429 0.048 Uiso 1 1 calc R . .
C22 C -0.1007(2) 0.8362(3) 0.55853(18) 0.0239(7) Uani 1 1 d . . .
C23 C -0.1141(2) 0.8657(3) 0.48790(19) 0.0276(8) Uani 1 1 d . . .
H23 H -0.1625 0.8909 0.4549 0.033 Uiso 1 1 calc R . .
C24 C -0.0426(2) 0.8504(3) 0.47668(17) 0.0242(7) Uani 1 1 d . . .
C25 C -0.0205(2) 0.8676(4) 0.41253(18) 0.0328(9) Uani 1 1 d . . .
H25A H -0.0667 0.8956 0.3746 0.049 Uiso 1 1 calc R . .
H25B H -0.0025 0.7912 0.3999 0.049 Uiso 1 1 calc R . .
H25C H 0.0217 0.9272 0.4218 0.049 Uiso 1 1 calc R . .
C31 C 0.2072(2) 0.8899(3) 0.84810(19) 0.0270(8) Uani 1 1 d . . .
C32 C 0.2604(2) 0.8792(4) 0.9171(2) 0.0350(9) Uani 1 1 d . . .
H32 H 0.262 0.8068 0.9417 0.042 Uiso 1 1 calc R . .
C33 C 0.3107(3) 0.9745(4) 0.9492(2) 0.0437(11) Uani 1 1 d . . .
H33 H 0.3454 0.9663 0.9952 0.052 Uiso 1 1 calc R . .
C34 C 0.3095(2) 1.0824(4) 0.9129(2) 0.0453(11) Uani 1 1 d . . .
H34 H 0.3438 1.1464 0.9343 0.054 Uiso 1 1 calc R . .
C35 C 0.2571(2) 1.0947(4) 0.8448(2) 0.0390(10) Uani 1 1 d . . .
H35 H 0.2561 1.1674 0.8206 0.047 Uiso 1 1 calc R . .
C36 C 0.2056(2) 0.9987(4) 0.81178(19) 0.0294(8) Uani 1 1 d . . .
H36 H 0.1706 1.0075 0.7659 0.035 Uiso 1 1 calc R . .
C41 C 0.2220(2) 0.6392(3) 0.82974(19) 0.0268(8) Uani 1 1 d . . .
C42 C 0.2675(2) 0.6308(4) 0.7854(2) 0.0348(9) Uani 1 1 d . . .
H42 H 0.254 0.6791 0.7453 0.042 Uiso 1 1 calc R . .
C43 C 0.3321(3) 0.5519(5) 0.8005(2) 0.0486(12) Uani 1 1 d . . .
H43 H 0.3633 0.5499 0.7718 0.058 Uiso 1 1 calc R . .
C44 C 0.3505(3) 0.4754(5) 0.8587(3) 0.0531(13) Uani 1 1 d . . .
H44 H 0.3928 0.4202 0.8681 0.064 Uiso 1 1 calc R . .
C45 C 0.3056(3) 0.4816(4) 0.9026(2) 0.0504(12) Uani 1 1 d . . .
H45 H 0.3179 0.4307 0.9416 0.06 Uiso 1 1 calc R . .
C46 C 0.2430(2) 0.5631(4) 0.88851(19) 0.0336(9) Uani 1 1 d . . .
H46 H 0.2139 0.5677 0.9189 0.04 Uiso 1 1 calc R . .
C51 C 0.0899(2) 0.7300(3) 0.87051(17) 0.0260(7) Uani 1 1 d . . .
C52 C 0.0581(2) 0.6152(4) 0.87597(19) 0.0301(8) Uani 1 1 d . . .
H52 H 0.0692 0.5488 0.8521 0.036 Uiso 1 1 calc R . .
C53 C 0.0100(2) 0.5995(4) 0.9171(2) 0.0367(9) Uani 1 1 d . . .
H53 H -0.0105 0.5224 0.9207 0.044 Uiso 1 1 calc R . .
C54 C -0.0076(2) 0.6973(4) 0.9524(2) 0.0412(10) Uani 1 1 d . . .
H54 H -0.04 0.6862 0.9796 0.049 Uiso 1 1 calc R . .
C55 C 0.0714(2) 0.8286(4) 0.90620(19) 0.0326(9) Uani 1 1 d . . .
H55 H 0.0915 0.9061 0.9026 0.039 Uiso 1 1 calc R . .
C56 C 0.0230(2) 0.8116(4) 0.9471(2) 0.0424(10) Uani 1 1 d . . .
H56 H 0.0114 0.8776 0.9709 0.051 Uiso 1 1 calc R . .
C60 C 0.1832(3) 0.8523(5) 0.3466(2) 0.0601(14) Uani 1 1 d . . .
H60A H 0.1257 0.8585 0.3225 0.072 Uiso 1 1 calc R . .
H60B H 0.2079 0.9255 0.3359 0.072 Uiso 1 1 calc R . .
C71 C -0.0784(2) 0.6323(3) 0.73033(19) 0.0285(8) Uani 1 1 d . . .
C72 C -0.1419(2) 0.5755(4) 0.7499(2) 0.0441(11) Uani 1 1 d . . .
H72A H -0.1291 0.4908 0.761 0.066 Uiso 1 1 calc R . .
H72B H -0.1918 0.5814 0.7114 0.066 Uiso 1 1 calc R . .
H72C H -0.1466 0.6167 0.7901 0.066 Uiso 1 1 calc R . .
C80 C 0.0755(3) 0.2047(4) 0.8502(2) 0.0529(12) Uani 1 1 d . . .
H80A H 0.0675 0.1302 0.8226 0.063 Uiso 1 1 calc R . .
H80B H 0.1143 0.2547 0.8385 0.063 Uiso 1 1 calc R . .
Cl1 Cl 0.00576(5) 0.95679(8) 0.73155(5) 0.0286(2) Uani 1 1 d . . .
Cl61 Cl 0.20279(7) 0.84545(11) 0.43722(6) 0.0501(3) Uani 1 1 d . . .
Cl62 Cl 0.21937(11) 0.72474(17) 0.31524(9) 0.0957(6) Uani 1 1 d . . .
Cl81 Cl -0.01603(8) 0.28436(13) 0.82728(9) 0.0717(4) Uani 1 1 d . . .
Cl82 Cl 0.11448(9) 0.16674(14) 0.93893(7) 0.0689(4) Uani 1 1 d . . .
N11 N 0.09286(17) 0.6228(3) 0.64695(14) 0.0233(6) Uani 1 1 d . . .
N12 N 0.10070(17) 0.6461(3) 0.58276(15) 0.0249(6) Uani 1 1 d . . .
N21 N -0.02348(17) 0.8054(3) 0.59007(14) 0.0229(6) Uani 1 1 d . . .
N22 N 0.01141(16) 0.8137(3) 0.53975(14) 0.0232(6) Uani 1 1 d . . .
N71 N -0.02802(17) 0.6779(3) 0.71641(15) 0.0255(6) Uani 1 1 d . . .
O1 O 0.14230(14) 0.8747(2) 0.66783(12) 0.0252(5) Uani 1 1 d . . .
O2 O 0.21077(14) 0.8957(2) 0.59418(13) 0.0302(6) Uani 1 1 d . . .
P1 P 0.14320(5) 0.75665(8) 0.80825(4) 0.02176(19) Uani 1 1 d . . .
Ru1 Ru 0.056566(16) 0.77249(3) 0.694338(14) 0.02021(8) Uani 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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 -1 4
3 -2 2
3 2 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
N12 C1 N22 109.7(3) . . ?
N12 C1 C2 110.6(3) . . ?
N22 C1 C2 112.4(3) . . ?
O2 C2 O1 125.5(3) . . ?
O2 C2 C1 117.6(3) . . ?
O1 C2 C1 116.8(3) . . ?
N11 C12 C13 110.3(3) . . ?
N11 C12 C11 122.5(3) . . ?
C13 C12 C11 127.2(3) . . ?
C14 C13 C12 107.1(3) . . ?
N12 C14 C13 105.9(3) . . ?
N12 C14 C15 123.5(3) . . ?
C13 C14 C15 130.6(3) . . ?
N21 C22 C23 109.4(3) . . ?
N21 C22 C21 122.7(3) . . ?
C23 C22 C21 127.9(3) . . ?
C24 C23 C22 107.3(3) . . ?
N22 C24 C23 105.6(3) . . ?
N22 C24 C25 123.0(3) . . ?
C23 C24 C25 131.4(3) . . ?
C36 C31 C32 118.9(3) . . ?
C36 C31 P1 122.8(3) . . ?
C32 C31 P1 118.3(3) . . ?
C33 C32 C31 121.0(4) . . ?
C32 C33 C34 120.0(4) . . ?
C35 C34 C33 119.8(4) . . ?
C34 C35 C36 120.7(4) . . ?
C31 C36 C35 119.6(4) . . ?
C46 C41 C42 117.8(3) . . ?
C46 C41 P1 125.2(3) . . ?
C42 C41 P1 116.8(3) . . ?
C43 C42 C41 120.9(4) . . ?
C42 C43 C44 119.9(4) . . ?
C45 C44 C43 119.9(4) . . ?
C46 C45 C44 119.9(4) . . ?
C45 C46 C41 121.5(4) . . ?
C52 C51 C55 118.6(3) . . ?
C52 C51 P1 120.8(3) . . ?
C55 C51 P1 120.0(3) . . ?
C53 C52 C51 120.3(4) . . ?
C54 C53 C52 120.6(4) . . ?
C53 C54 C56 119.6(4) . . ?
C56 C55 C51 120.4(4) . . ?
C54 C56 C55 120.4(4) . . ?
Cl62 C60 Cl61 112.5(3) . . ?
N71 C71 C72 178.5(4) . . ?
Cl82 C80 Cl81 113.3(3) . . ?
C12 N11 N12 105.1(3) . . ?
C12 N11 Ru1 138.2(2) . . ?
N12 N11 Ru1 115.6(2) . . ?
C14 N12 N11 111.6(3) . . ?
C14 N12 C1 128.9(3) . . ?
N11 N12 C1 119.5(3) . . ?
C22 N21 N22 106.0(3) . . ?
C22 N21 Ru1 137.6(2) . . ?
N22 N21 Ru1 115.8(2) . . ?
N21 N22 C24 111.6(3) . . ?
N21 N22 C1 118.3(3) . . ?
C24 N22 C1 129.7(3) . . ?
C71 N71 Ru1 174.7(3) . . ?
C2 O1 Ru1 120.4(2) . . ?
C41 P1 C51 104.73(16) . . ?
C41 P1 C31 98.24(16) . . ?
C51 P1 C31 101.87(16) . . ?
C41 P1 Ru1 118.84(12) . . ?
C51 P1 Ru1 112.24(11) . . ?
C31 P1 Ru1 118.51(12) . . ?
N71 Ru1 O1 177.88(11) . . ?
N71 Ru1 N11 94.07(11) . . ?
O1 Ru1 N11 86.27(10) . . ?
N71 Ru1 N21 90.84(11) . . ?
O1 Ru1 N21 87.12(10) . . ?
N11 Ru1 N21 83.20(11) . . ?
N71 Ru1 P1 91.69(9) . . ?
O1 Ru1 P1 90.30(7) . . ?
N11 Ru1 P1 101.37(8) . . ?
N21 Ru1 P1 174.60(8) . . ?
N71 Ru1 Cl1 88.41(9) . . ?
O1 Ru1 Cl1 90.96(7) . . ?
N11 Ru1 Cl1 171.55(8) . . ?
N21 Ru1 Cl1 88.70(8) . . ?
P1 Ru1 Cl1 86.60(3) . . ?
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 N12 1.453(4) . ?
C1 N22 1.458(4) . ?
C1 C2 1.533(5) . ?
C2 O2 1.235(4) . ?
C2 O1 1.279(4) . ?
C11 C12 1.502(5) . ?
C12 N11 1.335(4) . ?
C12 C13 1.404(5) . ?
C13 C14 1.368(5) . ?
C14 N12 1.365(4) . ?
C14 C15 1.502(5) . ?
C21 C22 1.496(5) . ?
C22 N21 1.339(4) . ?
C22 C23 1.407(5) . ?
C23 C24 1.372(5) . ?
C24 N22 1.369(4) . ?
C24 C25 1.493(5) . ?
C31 C36 1.394(5) . ?
C31 C32 1.399(5) . ?
C31 P1 1.851(4) . ?
C32 C33 1.379(6) . ?
C33 C34 1.387(7) . ?
C34 C35 1.382(6) . ?
C35 C36 1.400(5) . ?
C41 C46 1.395(5) . ?
C41 C42 1.401(5) . ?
C41 P1 1.836(4) . ?
C42 C43 1.380(6) . ?
C43 C44 1.391(7) . ?
C44 C45 1.383(6) . ?
C45 C46 1.374(6) . ?
C51 C52 1.394(5) . ?
C51 C55 1.397(5) . ?
C51 P1 1.841(3) . ?
C52 C53 1.392(5) . ?
C53 C54 1.380(6) . ?
C54 C56 1.380(6) . ?
C55 C56 1.394(5) . ?
C60 Cl62 1.742(5) . ?
C60 Cl61 1.753(5) . ?
C71 N71 1.138(4) . ?
C71 C72 1.454(5) . ?
C80 Cl82 1.742(5) . ?
C80 Cl81 1.756(5) . ?
Cl1 Ru1 2.4282(9) . ?
N11 N12 1.380(4) . ?
N11 Ru1 2.106(3) . ?
N21 N22 1.366(4) . ?
N21 Ru1 2.135(3) . ?
N71 Ru1 1.993(3) . ?
O1 Ru1 2.098(2) . ?
P1 Ru1 2.3011(10) . ?
