#------------------------------------------------------------------------------
#$Date: 2015-12-09 17:07:01 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171269 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/66/7036642.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_7036642
loop_
_publ_author_name
'Ng, Ho-Yuen'
'Cheung, Wai-Man'
'Kwan Huang, Enrique'
'Wong, Kang-Long'
'Sung, Herman H.-Y.'
'Williams, Ian D.'
'Leung, Wa-Hung'
_publ_section_title
;
 Ruthenium chalcogenonitrosyl and bridged nitrido complexes containing
 chelating sulfur and oxygen ligands.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18459
_journal_page_last               18468
_journal_paper_doi               10.1039/c5dt02513c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C48 H40 Cl N3 P4 Ru S5, H2 C Cl2'
_chemical_formula_sum            'C49 H42 Cl3 N3 P4 Ru S5'
_chemical_formula_weight         1164.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_audit_creation_date             2015-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-02 deposited with the CCDC.
2015-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3179(15)
_cell_length_b                   9.3685(10)
_cell_length_c                   18.4542(19)
_cell_measurement_reflns_used    4944
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.21
_cell_volume                     2473.9(4)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13642
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.771
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.855566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0286 before and 0.0169 after correction.
The Ratio of minimum to maximum transmission is 0.8556.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       needle
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5189
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0895P)²+10.8812P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4604
_reflns_number_total             5189
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02513c1.cif
_cod_data_source_block           vin43
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_source_target' value 'MO' changed to 'Mo' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7036640--7036645.cif.
;
_cod_database_code               7036642
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Cl4-C1SA = Cl2-C1S = Cl3-C1SA = Cl3-C1S
 1.72 with sigma of 0.02
3. Others
 Fixed Sof: Cl1(0.5) S1(0.5) N1(0.5) C1S(0.3) C1SA(0.2) Cl2(0.4) Cl3(0.5)
 Cl4(0.1)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H), C3(Ha), C4(Hb), C5(Hc), C6(Hd), C8(He), C9(Hf), C10(Hg), C11(Hh),
 C12(Hi), C14(Hj), C15(Hk), C16(Hl), C17(Hm), C18(Hn), C20(Ho), C21(Hp),
 C22(Hq), C23(Hr), C24(Hs)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection '18 Jan 2010'
_olex2_date_sample_submission    '17 Jan 2010'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_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 0.5000 1.0000 0.0000 0.01237(14) Uani 1 2 d S T P . .
Cl1 Cl 0.51673(18) 1.2348(4) 0.05057(16) 0.0188(6) Uani 0.5 1 d . . . A 2
S1 S 0.5344(2) 1.3117(4) 0.06956(18) 0.0381(7) Uani 0.5 1 d . . . A 1
S2 S 0.34836(7) 0.99329(11) 0.05515(6) 0.0186(2) Uani 1 1 d . . . . .
S3 S 0.59810(7) 0.90588(12) 0.09832(5) 0.0180(2) Uani 1 1 d . . . . .
P1 P 0.33468(7) 0.80439(11) 0.10750(5) 0.0141(2) Uani 1 1 d . . . . .
P2 P 0.51848(7) 0.81755(11) 0.17572(5) 0.0136(2) Uani 1 1 d . . . . .
N1 N 0.5165(6) 1.1706(12) 0.0361(5) 0.0152(17) Uani 0.5 1 d . . . A 1
N2 N 0.4246(2) 0.7407(4) 0.14963(19) 0.0169(7) Uani 1 1 d . . . . .
C1 C 0.2406(3) 0.8334(5) 0.1691(2) 0.0176(8) Uani 1 1 d . . . . .
C2 C 0.2316(3) 0.7375(5) 0.2255(2) 0.0227(9) Uani 1 1 d . . . . .
H2 H 0.2741 0.6600 0.2307 0.027 Uiso 1 1 calc R . . . .
C3 C 0.1608(3) 0.7536(6) 0.2747(2) 0.0288(11) Uani 1 1 d . . . . .
H3 H 0.1550 0.6877 0.3134 0.035 Uiso 1 1 calc R . . . .
C4 C 0.0985(3) 0.8670(6) 0.2667(3) 0.0302(11) Uani 1 1 d . . . . .
H4 H 0.0511 0.8800 0.3009 0.036 Uiso 1 1 calc R . . . .
C5 C 0.1053(3) 0.9612(5) 0.2091(3) 0.0286(11) Uani 1 1 d . . . . .
H5 H 0.0613 1.0364 0.2029 0.034 Uiso 1 1 calc R . . . .
C6 C 0.1768(3) 0.9456(5) 0.1602(2) 0.0227(9) Uani 1 1 d . . . . .
H6 H 0.1822 1.0108 0.1211 0.027 Uiso 1 1 calc R . . . .
C7 C 0.2909(3) 0.6626(5) 0.0486(2) 0.0173(8) Uani 1 1 d . . . . .
C8 C 0.3281(3) 0.5277(5) 0.0549(3) 0.0232(9) Uani 1 1 d . . . . .
H8 H 0.3794 0.5099 0.0877 0.028 Uiso 1 1 calc R . . . .
C9 C 0.2903(4) 0.4175(5) 0.0129(3) 0.0301(11) Uani 1 1 d . . . . .
H9 H 0.3160 0.3243 0.0170 0.036 Uiso 1 1 calc R . . . .
C10 C 0.2159(4) 0.4418(6) -0.0347(3) 0.0299(11) Uani 1 1 d . . . . .
H10 H 0.1905 0.3659 -0.0633 0.036 Uiso 1 1 calc R . . . .
C11 C 0.1781(3) 0.5783(6) -0.0406(2) 0.0274(10) Uani 1 1 d . . . . .
H11 H 0.1268 0.5957 -0.0735 0.033 Uiso 1 1 calc R . . . .
C12 C 0.2148(3) 0.6889(5) 0.0012(2) 0.0238(9) Uani 1 1 d . . . . .
H12 H 0.1885 0.7818 -0.0024 0.029 Uiso 1 1 calc R . . . .
C13 C 0.5005(3) 0.9408(5) 0.2488(2) 0.0177(8) Uani 1 1 d . . . . .
C14 C 0.5558(3) 1.0631(5) 0.2591(2) 0.0204(9) Uani 1 1 d . . . . .
H14 H 0.6016 1.0873 0.2252 0.025 Uiso 1 1 calc R . . . .
C15 C 0.5429(3) 1.1485(5) 0.3194(2) 0.0236(9) Uani 1 1 d . . . . .
H15 H 0.5796 1.2323 0.3261 0.028 Uiso 1 1 calc R . . . .
C16 C 0.4774(3) 1.1132(5) 0.3699(2) 0.0264(10) Uani 1 1 d . . . . .
H16 H 0.4701 1.1718 0.4113 0.032 Uiso 1 1 calc R . . . .
C17 C 0.4222(3) 0.9918(6) 0.3600(3) 0.0283(10) Uani 1 1 d . . . . .
H17 H 0.3766 0.9682 0.3942 0.034 Uiso 1 1 calc R . . . .
C18 C 0.4341(3) 0.9055(5) 0.3000(2) 0.0237(9) Uani 1 1 d . . . . .
H18 H 0.3971 0.8220 0.2935 0.028 Uiso 1 1 calc R . . . .
C19 C 0.5914(3) 0.6786(5) 0.2151(2) 0.0172(8) Uani 1 1 d . . . . .
C20 C 0.6130(4) 0.5623(6) 0.1723(3) 0.0345(12) Uani 1 1 d . . . . .
H20 H 0.5899 0.5580 0.1235 0.041 Uiso 1 1 calc R . . . .
C21 C 0.6682(4) 0.4517(6) 0.2003(3) 0.0401(14) Uani 1 1 d . . . . .
H21 H 0.6821 0.3722 0.1706 0.048 Uiso 1 1 calc R . . . .
C22 C 0.7028(3) 0.4564(5) 0.2707(3) 0.0283(11) Uani 1 1 d . . . . .
H22 H 0.7393 0.3798 0.2901 0.034 Uiso 1 1 calc R . . . .
C23 C 0.6839(4) 0.5737(6) 0.3126(3) 0.0313(11) Uani 1 1 d . . . . .
H23 H 0.7093 0.5792 0.3607 0.038 Uiso 1 1 calc R . . . .
C24 C 0.6287(3) 0.6837(5) 0.2856(3) 0.0265(10) Uani 1 1 d . . . . .
H24 H 0.6161 0.7635 0.3155 0.032 Uiso 1 1 calc R . . . .
C1S C 0.5670(16) 0.4612(19) 0.4740(12) 0.050(6) Uiso 0.3 1 d D . . B 1
C1SA C 0.532(2) 0.457(2) 0.4625(12) 0.037(7) Uiso 0.2 1 d D . . B 2
Cl2 Cl 0.4947(3) 0.6200(5) 0.4662(3) 0.0471(10) Uiso 0.4 1 d D . . B 1
Cl3 Cl 0.5319(3) 0.3372(5) 0.5375(2) 0.0591(10) Uiso 0.5 1 d D . . . .
Cl4 Cl 0.4623(13) 0.593(2) 0.4948(11) 0.054(4) Uiso 0.1 1 d D . . 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'
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
Cl1 Ru1 Cl1 180.00(12) . 3_675
Cl1 Ru1 S2 93.47(7) 3_675 .
Cl1 Ru1 S2 93.47(7) . 3_675
Cl1 Ru1 S2 86.53(7) . .
Cl1 Ru1 S2 86.53(7) 3_675 3_675
Cl1 Ru1 S3 90.30(7) . 3_675
Cl1 Ru1 S3 90.30(7) 3_675 .
Cl1 Ru1 S3 89.70(7) . .
Cl1 Ru1 S3 89.70(7) 3_675 3_675
S2 Ru1 S2 180.0 . 3_675
S3 Ru1 S2 79.61(3) 3_675 .
S3 Ru1 S2 100.39(3) . .
S3 Ru1 S2 100.38(3) 3_675 3_675
S3 Ru1 S2 79.62(3) . 3_675
S3 Ru1 S3 180.0 3_675 .
N1 Ru1 S2 88.6(3) 3_675 3_675
N1 Ru1 S2 91.4(3) . 3_675
N1 Ru1 S2 88.6(3) . .
N1 Ru1 S2 91.4(3) 3_675 .
N1 Ru1 S3 88.8(3) 3_675 3_675
N1 Ru1 S3 88.8(3) . .
N1 Ru1 S3 91.2(3) . 3_675
N1 Ru1 S3 91.2(3) 3_675 .
N1 Ru1 N1 180.0 3_675 .
P1 S2 Ru1 108.92(5) . .
P2 S3 Ru1 110.47(5) . .
N2 P1 S2 117.92(14) . .
N2 P1 C1 110.76(19) . .
N2 P1 C7 105.93(19) . .
C1 P1 S2 104.72(15) . .
C1 P1 C7 103.68(19) . .
C7 P1 S2 112.98(14) . .
N2 P2 S3 117.48(14) . .
N2 P2 C13 112.16(19) . .
N2 P2 C19 105.50(19) . .
C13 P2 S3 111.29(15) . .
C13 P2 C19 104.9(2) . .
C19 P2 S3 104.22(14) . .
S1 N1 Ru1 176.8(7) . .
P2 N2 P1 129.8(2) . .
C2 C1 P1 117.7(3) . .
C2 C1 C6 119.9(4) . .
C6 C1 P1 122.3(3) . .
C1 C2 C3 120.6(4) . .
C4 C3 C2 119.5(4) . .
C5 C4 C3 120.3(4) . .
C4 C5 C6 120.1(5) . .
C5 C6 C1 119.6(4) . .
C8 C7 P1 119.8(3) . .
C8 C7 C12 120.5(4) . .
C12 C7 P1 119.5(3) . .
C7 C8 C9 119.5(4) . .
C10 C9 C8 120.8(5) . .
C9 C10 C11 119.5(5) . .
C12 C11 C10 120.3(4) . .
C11 C12 C7 119.4(4) . .
C14 C13 P2 122.1(3) . .
C14 C13 C18 119.6(4) . .
C18 C13 P2 118.1(3) . .
C15 C14 C13 119.4(4) . .
C16 C15 C14 120.9(4) . .
C15 C16 C17 120.0(4) . .
C18 C17 C16 119.7(4) . .
C17 C18 C13 120.4(4) . .
C20 C19 P2 118.3(3) . .
C20 C19 C24 118.3(4) . .
C24 C19 P2 123.3(3) . .
C19 C20 C21 120.5(5) . .
C22 C21 C20 120.6(5) . .
C21 C22 C23 119.0(5) . .
C22 C23 C24 121.0(5) . .
C23 C24 C19 120.5(5) . .
Cl2 C1S Cl2 96.6(10) 3_666 .
Cl2 C1S Cl3 18.6(3) 3_666 .
Cl3 C1S Cl2 115.1(11) . .
C1SA C1SA Cl3 52.5(10) 3_666 3_666
Cl3 C1SA C1SA 71.4(11) . 3_666
Cl3 C1SA Cl3 123.9(11) . 3_666
Cl4 C1SA C1SA 67(2) 3_666 3_666
Cl4 C1SA C1SA 29.3(9) . 3_666
Cl4 C1SA Cl3 100.4(13) . .
Cl4 C1SA Cl3 9.6(16) 3_666 .
Cl4 C1SA Cl3 119(2) 3_666 3_666
Cl4 C1SA Cl3 23.9(8) . 3_666
Cl4 C1SA Cl4 97(2) 3_666 .
C1S Cl2 C1S 83.4(10) 3_666 .
Cl3 Cl2 C1S 171.1(12) 3_666 .
Cl3 Cl2 C1S 92.0(10) 3_666 3_666
C1SA Cl3 C1SA 56.1(11) . 3_666
Cl2 Cl3 C1S 69.3(10) 3_666 .
Cl4 Cl3 C1SA 10.0(16) 3_666 .
Cl4 Cl3 C1SA 52.2(12) 3_666 3_666
C1SA Cl4 C1SA 83(2) 3_666 .
C1SA Cl4 Cl4 57(2) 3_666 3_666
C1SA Cl4 Cl4 26.4(8) . 3_666
Cl3 Cl4 C1SA 103.9(17) 3_666 .
Cl3 Cl4 C1SA 160(3) 3_666 3_666
Cl3 Cl4 Cl4 129(2) 3_666 3_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 Cl1 2.398(4) .
Ru1 Cl1 2.398(4) 3_675
Ru1 S2 2.4301(10) 3_675
Ru1 S2 2.4301(10) .
Ru1 S3 2.4222(10) 3_675
Ru1 S3 2.4223(10) .
Ru1 N1 1.744(11) .
Ru1 N1 1.744(11) 3_675
S1 N1 1.478(11) .
S2 P1 2.0290(15) .
S3 P2 2.0337(14) .
P1 N2 1.596(4) .
P1 C1 1.813(4) .
P1 C7 1.815(4) .
P2 N2 1.585(4) .
P2 C13 1.800(4) .
P2 C19 1.805(4) .
C1 C2 1.384(6) .
C1 C6 1.399(6) .
C2 C3 1.392(6) .
C3 C4 1.392(8) .
C4 C5 1.388(7) .
C5 C6 1.395(6) .
C7 C8 1.375(6) .
C7 C12 1.395(6) .
C8 C9 1.390(7) .
C9 C10 1.375(7) .
C10 C11 1.392(8) .
C11 C12 1.384(7) .
C13 C14 1.402(6) .
C13 C18 1.403(6) .
C14 C15 1.387(6) .
C15 C16 1.385(7) .
C16 C17 1.394(7) .
C17 C18 1.387(6) .
C19 C20 1.387(7) .
C19 C24 1.391(6) .
C20 C21 1.393(7) .
C21 C22 1.375(8) .
C22 C23 1.376(8) .
C23 C24 1.381(7) .
C1S Cl2 1.815(16) .
C1S Cl2 1.626(18) 3_666
C1S Cl3 1.737(16) .
C1SA C1SA 1.87(4) 3_666
C1SA Cl3 1.784(17) .
C1SA Cl3 2.13(2) 3_666
C1SA Cl4 1.734(18) .
C1SA Cl4 0.92(2) 3_666
Cl2 C1S 1.626(18) 3_666
Cl2 Cl3 0.556(5) 3_666
Cl3 C1SA 2.13(2) 3_666
Cl3 Cl2 0.556(5) 3_666
Cl3 Cl4 0.89(2) 3_666
Cl4 C1SA 0.92(2) 3_666
Cl4 Cl3 0.89(2) 3_666
Cl4 Cl4 2.06(4) 3_666
