#------------------------------------------------------------------------------
#$Date: 2017-02-04 15:10:19 +0100 (Sat 04 de Feb de 2017) $
#$Revision: 191707 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/59/7055906.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_7055906
loop_
_publ_author_name
'Saha, Pinaki'
'Samanta, Debasish'
'Ghosh, Prasanta'
_publ_section_title
;
 Glyoxalbis(2-methylmercaptoanil) complexes of nickel and ruthenium:
 radical versus non-radical states
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              1149
_journal_paper_doi               10.1039/C6NJ02903E
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C34 H31 Cl N2 P Ru S2, Cl, H2 O'
_chemical_formula_sum            'C34 H33 Cl2 N2 O P Ru S2'
_chemical_formula_weight         752.68
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-08-04 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.963(5)
_cell_length_b                   19.963(5)
_cell_length_c                   15.819(5)
_cell_measurement_reflns_used    9468
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      2.35
_cell_volume                     5460(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32957
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         1.745
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker AXS Inc. 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       prism
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4313
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.1012P)²+4.4103P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3265
_reflns_number_total             4313
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6nj02903e2.cif
_cod_data_source_block           3Cl_H2O
_cod_depositor_comments
'Adding full bibliography for 7055903--7055906.cif.'
_cod_database_code               7055906
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.692
_shelx_estimated_absorpt_t_max   0.850
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.65569(2) 0.56816(2) 0.7500 0.04934(18) Uani 1 2 d S T P A .
Cl1 Cl 0.55776(9) 0.42976(9) 0.7500 0.0656(4) Uani 1 2 d S T P . .
C1 C 0.6953(4) 0.4553(3) 0.6093(3) 0.0911(16) Uani 1 1 d . . . . .
H1A H 0.6417 0.4189 0.6197 0.137 Uiso 1 1 calc R U . . .
H1B H 0.7268 0.4452 0.6469 0.137 Uiso 1 1 calc R U . . .
H1C H 0.7078 0.4504 0.5518 0.137 Uiso 1 1 calc R U . . .
S2 S 0.71320(6) 0.55286(6) 0.62690(7) 0.0587(3) Uani 1 1 d . . . . .
C3 C 0.6499(2) 0.5608(2) 0.5523(3) 0.0581(10) Uani 1 1 d . . . . .
C4 C 0.6583(3) 0.5536(3) 0.4670(3) 0.0723(12) Uani 1 1 d . . . . .
H4 H 0.6930 0.5386 0.4479 0.087 Uiso 1 1 calc R U . . .
C5 C 0.6155(3) 0.5686(3) 0.4100(3) 0.0858(15) Uani 1 1 d . . . . .
H5 H 0.6209 0.5630 0.3525 0.103 Uiso 1 1 calc R U . . .
C6 C 0.5654(3) 0.5914(3) 0.4368(3) 0.0847(15) Uani 1 1 d . . . . .
H6 H 0.5379 0.6026 0.3972 0.102 Uiso 1 1 calc R U . . .
C7 C 0.5546(3) 0.5983(3) 0.5222(3) 0.0752(12) Uani 1 1 d . . . . .
H7 H 0.5203 0.6141 0.5403 0.090 Uiso 1 1 calc R U . . .
C8 C 0.5958(2) 0.5811(2) 0.5803(3) 0.0607(9) Uani 1 1 d . . . . .
N9 N 0.58707(18) 0.58356(19) 0.6690(2) 0.0567(7) Uani 1 1 d . . . . .
C10 C 0.5320(3) 0.5904(3) 0.7047(3) 0.0684(11) Uani 1 1 d . . . . .
H10 H 0.4951 0.5950 0.6734 0.082 Uiso 1 1 calc R U . . .
P1 P 0.74969(9) 0.69811(9) 0.7500 0.0565(4) Uani 1 2 d S T P . .
C11 C 0.8513(4) 0.7215(4) 0.7500 0.0699(16) Uani 1 2 d S TU P A .
C12 C 0.9085(5) 0.7979(6) 0.7500 0.115(3) Uani 1 2 d S TU P . .
H12 H 0.8966 0.8374 0.7500 0.138 Uiso 1 2 calc R U P A .
C13 C 0.9898(6) 0.8151(7) 0.7500 0.133(4) Uani 1 2 d S TU P A .
H13 H 1.0304 0.8660 0.7500 0.160 Uiso 1 2 calc R U P . .
C14 C 1.0045(6) 0.7546(7) 0.7500 0.119(3) Uani 1 2 d S TU P . .
H14 H 1.0555 0.7652 0.7500 0.143 Uiso 1 2 calc R U P A .
C15 C 0.9468(4) 0.6806(6) 0.7500 0.090(2) Uani 1 2 d S TU P A .
H15 H 0.9582 0.6407 0.7500 0.108 Uiso 1 2 calc R U P . .
C16 C 0.8714(3) 0.6636(4) 0.7500 0.0663(15) Uani 1 2 d S TU P . .
H16 H 0.8323 0.6121 0.7500 0.080 Uiso 1 2 calc R U P A .
C21 C 0.7424(6) 0.7484(6) 0.8441(4) 0.0758(15) Uani 0.678(15) 1 d G U P A 1
C22 C 0.7791(6) 0.7435(5) 0.9166(5) 0.088(2) Uani 0.678(15) 1 d G U P A 1
H22 H 0.8146 0.7263 0.9129 0.106 Uiso 0.678(15) 1 calc R U P A 1
C23 C 0.7628(7) 0.7643(6) 0.9945(4) 0.111(3) Uani 0.678(15) 1 d G U P A 1
H23 H 0.7874 0.7611 1.0430 0.133 Uiso 0.678(15) 1 calc R U P A 1
C24 C 0.7098(7) 0.7900(6) 0.9999(6) 0.134(4) Uani 0.678(15) 1 d G U P A 1
H24 H 0.6990 0.8039 1.0521 0.161 Uiso 0.678(15) 1 calc R U P A 1
C25 C 0.6731(6) 0.7949(7) 0.9275(8) 0.140(4) Uani 0.678(15) 1 d G U P A 1
H25 H 0.6376 0.8121 0.9312 0.168 Uiso 0.678(15) 1 calc R U P A 1
C26 C 0.6894(7) 0.7741(8) 0.8496(6) 0.121(4) Uani 0.678(15) 1 d G U P A 1
H26 H 0.6648 0.7773 0.8011 0.145 Uiso 0.678(15) 1 calc R U P A 1
C21' C 0.7497(13) 0.7486(14) 0.8457(9) 0.0758(15) Uani 0.322(15) 1 d G U P A 2
C22' C 0.8093(12) 0.7659(11) 0.9026(11) 0.088(2) Uani 0.322(15) 1 d G U P A 2
H22' H 0.8506 0.7596 0.8868 0.106 Uiso 0.322(15) 1 calc R U P A 2
C23' C 0.8070(14) 0.7927(12) 0.9830(10) 0.111(3) Uani 0.322(15) 1 d G U P A 2
H23' H 0.8468 0.8042 1.0211 0.133 Uiso 0.322(15) 1 calc R U P A 2
C24' C 0.7451(15) 0.8021(13) 1.0066(12) 0.134(4) Uani 0.322(15) 1 d G U P A 2
H24' H 0.7436 0.8200 1.0605 0.161 Uiso 0.322(15) 1 calc R U P A 2
C25' C 0.6856(13) 0.7848(17) 0.9497(18) 0.140(4) Uani 0.322(15) 1 d G U P A 2
H25' H 0.6442 0.7912 0.9655 0.168 Uiso 0.322(15) 1 calc R U P A 2
C26' C 0.6879(13) 0.7581(18) 0.8693(16) 0.121(4) Uani 0.322(15) 1 d G U P A 2
H26' H 0.6480 0.7465 0.8312 0.145 Uiso 0.322(15) 1 calc R U P A 2
Cl2 Cl 0.4323(3) 0.6766(3) 0.6013(3) 0.1402(15) Uani 0.5 1 d . . P . .
O30 O 0.5379(6) 0.7922(5) 0.7500 0.112(3) Uani 0.727(11) 2 d S T P B 1
O30' O 0.4797(17) 0.7980(14) 0.7500 0.112(3) Uani 0.273(11) 2 d S T P B 2
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'
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 0.0060 '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'
S S 0.1246 0.1234 '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
N9 Ru1 N9 79.27(19) . 10_557
N9 Ru1 P1 93.50(10) . .
N9 Ru1 P1 93.50(10) 10_557 .
N9 Ru1 S2 163.88(10) . 10_557
N9 Ru1 S2 84.63(10) 10_557 10_557
P1 Ru1 S2 88.33(3) . 10_557
N9 Ru1 S2 84.63(10) . .
N9 Ru1 S2 163.88(10) 10_557 .
P1 Ru1 S2 88.33(3) . .
S2 Ru1 S2 111.44(6) 10_557 .
N9 Ru1 Cl1 87.25(10) . .
N9 Ru1 Cl1 87.25(10) 10_557 .
P1 Ru1 Cl1 179.02(6) . .
S2 Ru1 Cl1 91.12(4) 10_557 .
S2 Ru1 Cl1 91.12(4) . .
S2 C1 H1A 109.5 . .
S2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
S2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 S2 C1 102.9(2) . .
C3 S2 Ru1 96.99(15) . .
C1 S2 Ru1 114.71(19) . .
C4 C3 C8 119.5(4) . .
C4 C3 S2 120.5(4) . .
C8 C3 S2 119.8(3) . .
C5 C4 C3 119.9(5) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C6 C5 C4 120.8(5) . .
C6 C5 H5 119.6 . .
C4 C5 H5 119.6 . .
C5 C6 C7 120.9(5) . .
C5 C6 H6 119.6 . .
C7 C6 H6 119.6 . .
C8 C7 C6 118.8(5) . .
C8 C7 H7 120.6 . .
C6 C7 H7 120.6 . .
C7 C8 C3 120.0(4) . .
C7 C8 N9 123.3(4) . .
C3 C8 N9 116.6(4) . .
C10 N9 C8 123.9(4) . .
C10 N9 Ru1 114.6(3) . .
C8 N9 Ru1 121.4(3) . .
N9 C10 C10 115.7(2) . 10_557
N9 C10 H10 122.1 . .
C10 C10 H10 122.1 10_557 .
C21' P1 C21' 112.7(16) . 10_557
C21' P1 C11 99.5(7) . .
C21' P1 C11 99.5(7) 10_557 .
C11 P1 C21 103.9(3) . 10_557
C11 P1 C21 103.9(3) . .
C21 P1 C21 107.9(7) 10_557 .
C21' P1 Ru1 113.3(7) . .
C21' P1 Ru1 113.3(7) 10_557 .
C11 P1 Ru1 117.2(2) . .
C21 P1 Ru1 111.7(3) 10_557 .
C21 P1 Ru1 111.6(3) . .
C12 C11 C16 119.6(7) . .
C12 C11 P1 118.7(6) . .
C16 C11 P1 121.7(5) . .
C11 C12 C13 117.6(10) . .
C11 C12 H12 121.2 . .
C13 C12 H12 121.2 . .
C14 C13 C12 119.0(10) . .
C14 C13 H13 120.5 . .
C12 C13 H13 120.5 . .
C15 C14 C13 121.5(9) . .
C15 C14 H14 119.2 . .
C13 C14 H14 119.2 . .
C14 C15 C16 120.3(9) . .
C14 C15 H15 119.9 . .
C16 C15 H15 119.9 . .
C15 C16 C11 122.0(7) . .
C15 C16 H16 119.0 . .
C11 C16 H16 119.0 . .
C22 C21 C26 120.0 . .
C22 C21 P1 116.1(6) . .
C26 C21 P1 122.3(6) . .
C23 C22 C21 120.0 . .
C23 C22 H22 120.0 . .
C21 C22 H22 120.0 . .
C24 C23 C22 120.0 . .
C24 C23 H23 120.0 . .
C22 C23 H23 120.0 . .
C23 C24 C25 120.0 . .
C23 C24 H24 120.0 . .
C25 C24 H24 120.0 . .
C26 C25 C24 120.0 . .
C26 C25 H25 120.0 . .
C24 C25 H25 120.0 . .
C25 C26 C21 120.0 . .
C25 C26 H26 120.0 . .
C21 C26 H26 120.0 . .
C22' C21' C26' 120.0 . .
C22' C21' P1 116.1(13) . .
C26' C21' P1 123.0(12) . .
C23' C22' C21' 120.0 . .
C23' C22' H22' 120.0 . .
C21' C22' H22' 120.0 . .
C22' C23' C24' 120.0 . .
C22' C23' H23' 120.0 . .
C24' C23' H23' 120.0 . .
C25' C24' C23' 120.0 . .
C25' C24' H24' 120.0 . .
C23' C24' H24' 120.0 . .
C26' C25' C24' 120.0 . .
C26' C25' H25' 120.0 . .
C24' C25' H25' 120.0 . .
C25' C26' C21' 120.0 . .
C25' C26' H26' 120.0 . .
C21' C26' H26' 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N9 2.008(3) .
Ru1 N9 2.008(3) 10_557
Ru1 P1 2.3202(17) .
Ru1 S2 2.3566(12) 10_557
Ru1 S2 2.3567(12) .
Ru1 Cl1 2.4606(17) .
C1 S2 1.816(5) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
S2 C3 1.793(4) .
C3 C4 1.377(6) .
C3 C8 1.401(6) .
C4 C5 1.374(8) .
C4 H4 0.9300 .
C5 C6 1.359(8) .
C5 H5 0.9300 .
C6 C7 1.386(7) .
C6 H6 0.9300 .
C7 C8 1.385(6) .
C7 H7 0.9300 .
C8 N9 1.418(5) .
N9 C10 1.303(5) .
C10 C10 1.432(9) 10_557
C10 H10 0.9300 .
P1 C21' 1.818(17) .
P1 C21' 1.818(17) 10_557
P1 C11 1.839(6) .
P1 C21 1.842(8) 10_557
P1 C21 1.842(8) .
C11 C12 1.374(11) .
C11 C16 1.400(9) .
C12 C13 1.483(14) .
C12 H12 0.9300 .
C13 C14 1.378(15) .
C13 H13 0.9300 .
C14 C15 1.346(13) .
C14 H14 0.9300 .
C15 C16 1.368(9) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C21 C22 1.3900 .
C21 C26 1.3900 .
C22 C23 1.3900 .
C22 H22 0.9300 .
C23 C24 1.3900 .
C23 H23 0.9300 .
C24 C25 1.3900 .
C24 H24 0.9300 .
C25 C26 1.3900 .
C25 H25 0.9300 .
C26 H26 0.9300 .
C21' C22' 1.3900 .
C21' C26' 1.3900 .
C22' C23' 1.3900 .
C22' H22' 0.9300 .
C23' C24' 1.3900 .
C23' H23' 0.9300 .
C24' C25' 1.3900 .
C24' H24' 0.9300 .
C25' C26' 1.3900 .
C25' H25' 0.9300 .
C26' H26' 0.9300 .
