#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/53/7035375.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_7035375
loop_
_publ_author_name
'Płotek, Michał'
'Starosta, Radosław'
'Komarnicka, Urszula K.'
'Skórska-Stania, Agnieszka'
'Jeżowska-Bojczuk, Małgorzata'
'Stochel, Grażyna'
'Kyzioł, Agnieszka'
_publ_section_title
;
 New ruthenium(ii) coordination compounds possessing bidentate
 aminomethylphosphane ligands: synthesis, characterization and preliminary
 biological study in vitro.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13969
_journal_page_last               13978
_journal_paper_doi               10.1039/c5dt01119a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C38 H46 Cl2 N4 O2 P2 Ru, 2(C2 H3 N)'
_chemical_formula_sum            'C42 H52 Cl2 N6 O2 P2 Ru'
_chemical_formula_weight         906.8
_chemical_name_systematic
(OC-6-33)-bis(acetonitrile)dichlorobis{[4-(tetrahydro-1,4-oxazino)methyl]diphenylphosphine-?P}ruthenium(II)
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-14T06:35:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-05-07 deposited with the CCDC.
2015-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.725(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7701(3)
_cell_length_b                   15.4658(4)
_cell_length_c                   23.8880(5)
_cell_measurement_reflns_used    4757
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.82
_cell_measurement_theta_min      3.02
_cell_measurement_wavelength     0.71073
_cell_volume                     4257.70(18)
_computing_cell_refinement
'CrysalisPro  Version 1.171.33.66 (Agilent Technologies, 2010)'
_computing_data_collection
'CrysalisPro  Version 1.171.33.66 (Agilent Technologies, 2010)'
_computing_data_reduction
'CrysalisPro  Version 1.171.33.66 (Agilent Technologies, 2010)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_details
;
  1 omega  -91.00    9.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2777  -77.0000 -150.0000 100

  2 omega   35.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0277  178.0000  120.0000 72

;
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_orient_matrix_UB_11      -0.0608788000
_diffrn_orient_matrix_UB_12      -0.0006239000
_diffrn_orient_matrix_UB_13      -0.0018016000
_diffrn_orient_matrix_UB_21      0.0008781000
_diffrn_orient_matrix_UB_22      0.0450350000
_diffrn_orient_matrix_UB_23      0.0056853000
_diffrn_orient_matrix_UB_31      -0.0089236000
_diffrn_orient_matrix_UB_32      0.0086529000
_diffrn_orient_matrix_UB_33      -0.0297416000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.039
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9470
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.893
_diffrn_reflns_theta_min         3.024
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.11
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0465P)²+7.7969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0
_reflns_number_gt                5071
_reflns_number_total             6038
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01119a2.cif
_cod_data_source_block           rupm1a
_cod_depositor_comments
'Adding full bibliography for 7035374--7035378.cif.'
_cod_original_cell_volume        4257.69(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7035375
#BEGIN Tags that were not found in dictionaries:
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.97
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ru1 Ru 0.5 0.60650(2) 0.75 0.01667(7) Uani 1 2 d S T P
P1 P 0.48571(5) 0.60934(3) 0.84694(2) 0.01554(11) Uani 1 1 d . . .
Cl1 Cl 0.64986(6) 0.71670(4) 0.76798(2) 0.03181(15) Uani 1 1 d . . .
N4 N 0.3742(2) 0.51817(14) 0.73269(8) 0.0288(5) Uani 1 1 d . . .
C21 C 0.35445(19) 0.55580(15) 0.85905(9) 0.0192(4) Uani 1 1 d . . .
C31 C 0.60459(19) 0.56047(14) 0.89835(9) 0.0175(4) Uani 1 1 d . . .
C22 C 0.2544(2) 0.60180(17) 0.86241(11) 0.0262(5) Uani 1 1 d . . .
H22 H 0.2559 0.6619 0.8624 0.031 Uiso 1 1 calc R U .
C26 C 0.3489(2) 0.46533(15) 0.85739(9) 0.0230(5) Uani 1 1 d . . .
H26 H 0.4146 0.4335 0.8546 0.028 Uiso 1 1 calc R U .
C34 C 0.7957(2) 0.50289(15) 0.97951(10) 0.0229(4) Uani 1 1 d . . .
H34 H 0.8591 0.4842 1.0067 0.028 Uiso 1 1 calc R U .
C32 C 0.7182(2) 0.57874(15) 0.89213(9) 0.0204(4) Uani 1 1 d . . .
H32 H 0.7302 0.6102 0.8607 0.025 Uiso 1 1 calc R U .
C25 C 0.2459(2) 0.42264(18) 0.85996(10) 0.0291(5) Uani 1 1 d . . .
H25 H 0.2431 0.3626 0.8587 0.035 Uiso 1 1 calc R U .
C36 C 0.5884(2) 0.51217(15) 0.94561(9) 0.0198(4) Uani 1 1 d . . .
H36 H 0.5137 0.4991 0.9502 0.024 Uiso 1 1 calc R U .
C33 C 0.8128(2) 0.55018(15) 0.93255(10) 0.0229(4) Uani 1 1 d . . .
H33 H 0.8878 0.5628 0.9281 0.028 Uiso 1 1 calc R U .
C23 C 0.1523(2) 0.5590(2) 0.86575(12) 0.0349(6) Uani 1 1 d . . .
H23 H 0.0866 0.5904 0.8689 0.042 Uiso 1 1 calc R U .
C24 C 0.1480(2) 0.4693(2) 0.86433(12) 0.0346(6) Uani 1 1 d . . .
H24 H 0.0794 0.4407 0.8663 0.042 Uiso 1 1 calc R U .
C41 C 0.2931(3) 0.47511(19) 0.72131(11) 0.0382(7) Uani 1 1 d . . .
C42 C 0.1853(3) 0.4246(2) 0.70521(14) 0.0523(9) Uani 1 1 d . . .
H42A H 0.1227 0.4555 0.7163 0.079 Uiso 1 1 calc R U .
H42B H 0.1949 0.3697 0.7243 0.079 Uiso 1 1 calc R U .
H42C H 0.1681 0.4158 0.6646 0.079 Uiso 1 1 calc R U .
N1 N 0.47759(15) 0.72081(12) 0.93812(7) 0.0168(3) Uani 1 1 d . . .
C1 C 0.4801(2) 0.71929(14) 0.87698(9) 0.0183(4) Uani 1 1 d . . .
H1A H 0.5472 0.7516 0.871 0.022 Uiso 1 1 calc R U .
H1B H 0.4114 0.7485 0.8561 0.022 Uiso 1 1 calc R U .
C35 C 0.6839(2) 0.48345(16) 0.98595(10) 0.0228(4) Uani 1 1 d . . .
H35 H 0.6726 0.4512 1.0172 0.027 Uiso 1 1 calc R U .
C11 C 0.59216(18) 0.73722(15) 0.97422(9) 0.0192(4) Uani 1 1 d . . .
H11A H 0.6192 0.7941 0.9659 0.023 Uiso 1 1 calc R U .
H11B H 0.6473 0.6948 0.966 0.023 Uiso 1 1 calc R U .
O1 O 0.50251(14) 0.79233(11) 1.05051(7) 0.0235(3) Uani 1 1 d . . .
C14 C 0.39616(19) 0.78528(15) 0.95219(9) 0.0200(4) Uani 1 1 d . . .
H14A H 0.3195 0.7758 0.9289 0.024 Uiso 1 1 calc R U .
H14B H 0.4214 0.8429 0.9444 0.024 Uiso 1 1 calc R U .
C13 C 0.39160(19) 0.77725(16) 1.01494(9) 0.0218(4) Uani 1 1 d . . .
H13A H 0.3363 0.8187 1.0242 0.026 Uiso 1 1 calc R U .
H13B H 0.3651 0.7198 1.0223 0.026 Uiso 1 1 calc R U .
C12 C 0.5848(2) 0.73203(16) 1.03661(9) 0.0226(4) Uani 1 1 d . . .
H12A H 0.5626 0.6739 1.0452 0.027 Uiso 1 1 calc R U .
H12B H 0.6607 0.7438 1.0601 0.027 Uiso 1 1 calc R U .
N1A N 0.3713(4) 0.3157(3) 0.6511(2) 0.0880(13) Uani 1 1 d . . .
C1A C 0.4573(4) 0.2821(3) 0.6716(2) 0.0729(13) Uani 1 1 d . . .
C2A C 0.5601(5) 0.2398(5) 0.6872(3) 0.104(2) Uani 1 1 d . . .
H2A1 H 0.5712 0.2024 0.6567 0.157 Uiso 1 1 calc R U .
H2A2 H 0.5595 0.206 0.7208 0.157 Uiso 1 1 calc R U .
H2A3 H 0.6222 0.281 0.695 0.157 Uiso 1 1 calc R U .
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_
_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
N4 Ru1 N4 93.59(14) . 2_656
N4 Ru1 P1 91.04(6) . .
N4 Ru1 P1 90.42(6) 2_656 .
N4 Ru1 P1 90.42(6) . 2_656
N4 Ru1 P1 91.04(6) 2_656 2_656
P1 Ru1 P1 177.86(3) . 2_656
N4 Ru1 Cl1 87.82(7) . 2_656
N4 Ru1 Cl1 177.96(6) 2_656 2_656
P1 Ru1 Cl1 88.075(19) . 2_656
P1 Ru1 Cl1 90.425(19) 2_656 2_656
N4 Ru1 Cl1 177.96(6) . .
N4 Ru1 Cl1 87.82(7) 2_656 .
P1 Ru1 Cl1 90.43(2) . .
P1 Ru1 Cl1 88.07(2) 2_656 .
Cl1 Ru1 Cl1 90.81(4) 2_656 .
C31 P1 C21 105.24(10) . .
C31 P1 C1 101.68(10) . .
C21 P1 C1 104.87(10) . .
C31 P1 Ru1 117.06(7) . .
C21 P1 Ru1 112.25(7) . .
C1 P1 Ru1 114.41(7) . .
C41 N4 Ru1 172.2(3) . .
C22 C21 C26 118.5(2) . .
C22 C21 P1 122.01(18) . .
C26 C21 P1 118.96(17) . .
C36 C31 C32 118.8(2) . .
C36 C31 P1 123.51(17) . .
C32 C31 P1 117.47(16) . .
C23 C22 C21 120.8(2) . .
C25 C26 C21 120.5(2) . .
C33 C34 C35 120.0(2) . .
C33 C32 C31 120.6(2) . .
C24 C25 C26 120.2(2) . .
C35 C36 C31 120.3(2) . .
C34 C33 C32 120.1(2) . .
C24 C23 C22 120.2(3) . .
C25 C24 C23 119.8(2) . .
N4 C41 C42 176.5(4) . .
C1 N1 C11 112.72(17) . .
C1 N1 C14 112.62(17) . .
C11 N1 C14 108.21(16) . .
N1 C1 P1 114.20(15) . .
C34 C35 C36 120.2(2) . .
N1 C11 C12 109.90(17) . .
C13 O1 C12 109.66(16) . .
N1 C14 C13 109.06(18) . .
O1 C13 C14 111.35(17) . .
O1 C12 C11 111.76(19) . .
N1A C1A C2A 171.0(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N4 1.996(2) .
Ru1 N4 1.996(2) 2_656
Ru1 P1 2.3561(5) .
Ru1 P1 2.3562(5) 2_656
Ru1 Cl1 2.4274(6) 2_656
Ru1 Cl1 2.4274(6) .
P1 C31 1.827(2) .
P1 C21 1.827(2) .
P1 C1 1.852(2) .
N4 C41 1.150(4) .
C21 C22 1.392(3) .
C21 C26 1.401(3) .
C31 C36 1.399(3) .
C31 C32 1.403(3) .
C22 C23 1.389(4) .
C26 C25 1.392(3) .
C34 C33 1.388(3) .
C34 C35 1.389(3) .
C32 C33 1.390(3) .
C25 C24 1.382(4) .
C36 C35 1.396(3) .
C23 C24 1.388(4) .
C41 C42 1.473(4) .
N1 C1 1.467(3) .
N1 C11 1.468(3) .
N1 C14 1.469(3) .
C11 C12 1.512(3) .
O1 C13 1.425(3) .
O1 C12 1.432(3) .
C14 C13 1.516(3) .
N1A C1A 1.155(6) .
C1A C2A 1.359(8) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C31 P1 C21 C22 134.62(19)
C1 P1 C21 C22 27.8(2)
Ru1 P1 C21 C22 -96.99(18)
C31 P1 C21 C26 -53.97(19)
C1 P1 C21 C26 -160.79(17)
Ru1 P1 C21 C26 74.41(18)
C21 P1 C31 C36 -16.0(2)
C1 P1 C31 C36 93.11(19)
Ru1 P1 C31 C36 -141.47(16)
C21 P1 C31 C32 169.28(17)
C1 P1 C31 C32 -81.59(18)
Ru1 P1 C31 C32 43.83(19)
C26 C21 C22 C23 1.9(3)
P1 C21 C22 C23 173.3(2)
C22 C21 C26 C25 -1.0(3)
P1 C21 C26 C25 -172.70(17)
C36 C31 C32 C33 -0.7(3)
P1 C31 C32 C33 174.24(17)
C21 C26 C25 C24 -0.2(3)
C32 C31 C36 C35 0.5(3)
P1 C31 C36 C35 -174.12(17)
C35 C34 C33 C32 0.5(3)
C31 C32 C33 C34 0.2(3)
C21 C22 C23 C24 -1.6(4)
C26 C25 C24 C23 0.5(4)
C22 C23 C24 C25 0.4(4)
C11 N1 C1 P1 98.68(19)
C14 N1 C1 P1 -138.53(16)
C31 P1 C1 N1 -49.67(17)
C21 P1 C1 N1 59.76(17)
Ru1 P1 C1 N1 -176.82(12)
C33 C34 C35 C36 -0.7(4)
C31 C36 C35 C34 0.2(3)
C1 N1 C11 C12 -176.26(18)
C14 N1 C11 C12 58.5(2)
C1 N1 C14 C13 175.25(18)
C11 N1 C14 C13 -59.5(2)
C12 O1 C13 C14 -58.4(2)
N1 C14 C13 O1 60.5(2)
C13 O1 C12 C11 57.1(2)
N1 C11 C12 O1 -58.1(2)
