Ruthenium chalcogenonitrosyl and bridged nitrido complexes containing chelating sulfur and oxygen ligands.
Ng, Ho-Yuen; Cheung, Wai-Man; Kwan Huang, Enrique; Wong, Kang-Long; Sung, Herman H.-Y.; Williams, Ian D.; Leung, Wa-Hung; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18459–18468; doi:10.1039/c5dt02513c

data_7036644
_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_absolute_configuration ad
_chemical_formula_moiety         'C17 H30 Cl2 Co N O9 P3 Ru Se'
_chemical_formula_sum            'C17 H30 Cl2 Co N O9 P3 Ru Se'
_chemical_formula_weight         795.19
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.40074(14)
_cell_length_b                   15.56830(18)
_cell_length_c                   13.23672(14)
_cell_measurement_reflns_used    5786
_cell_measurement_temperature    203.01(10)
_cell_measurement_theta_max      75.2530
_cell_measurement_theta_min      5.3500
_cell_volume                     2967.61(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      203.01(10)
_diffrn_detector_area_resol_mean 10.3587
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   37.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000   30.0000 52

  2 omega  -27.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453   37.0000  -60.0000 57

  3 omega  -66.00   21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453   19.0000 -120.0000 87

  4 omega   38.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -180.0000 51

  5 omega   33.00   81.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000   90.0000 48

  6 omega   50.00   87.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -90.0000 37

  7 omega   36.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000 -120.0000 62

  8 omega   15.00   41.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7562  -99.0000    0.0000 26

  9 omega   57.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0703 -125.0000 -120.0000 41

 10 omega   87.00  173.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   45.0000 -180.0000 86

 11 omega   58.00  113.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000 -120.0000 55
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0353257000
_diffrn_orient_matrix_UB_12      0.0795452000
_diffrn_orient_matrix_UB_13      -0.0576348000
_diffrn_orient_matrix_UB_21      -0.0834097000
_diffrn_orient_matrix_UB_22      0.0063023000
_diffrn_orient_matrix_UB_23      0.0725403000
_diffrn_orient_matrix_UB_31      0.0568666000
_diffrn_orient_matrix_UB_32      0.0585602000
_diffrn_orient_matrix_UB_33      0.0704421000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9310
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.46
_diffrn_reflns_theta_min         4.18
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    13.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.030(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4355
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                4109
_reflns_number_total             4355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02513c1.cif
_cod_data_source_block           wai140a
_cod_depositor_comments
'Adding full bibliography for 7036640--7036645.cif.'
_cod_database_code               7036644
_chemical_oxdiff_formula         'Ce1 Co1 Cp1 Et6 O9 P3'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-C17 = C20-C19 = C16-C15 = C14-C13 = C12-C11
 1.52 with sigma of 0.015
 O6-C21 = O6-C21A
 1.43 with sigma of 0.015
 C22-C21 = C22A-C21A
 1.52 with sigma of 0.015
3. Others
 Fixed Sof: C21(0.5) C22(0.5) C21A(0.5) C22A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C)
;
_olex2_date_sample_data_collection 1406862399.0
_olex2_submission_special_instructions 'No special instructions were received'