Organo Ruthenium–Nickel Dithiolates with Redox-Responsive Nickel Sites
Chambers, Geoffrey M.; Angamuthu, Raja; Gray, Danielle L.; Rauchfuss, Thomas B.; Organometallics 32 (2013) 6324–; doi:10.1021/om4006824

data_4081855
_publ_section_title
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 Organo Ruthenium--Nickel Dithiolates with Redox-Responsive Nickel Sites
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_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6324
_journal_paper_doi               10.1021/om4006824
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C39 H68 Ni P2 Ru S2'
_chemical_formula_sum            'C39 H68 Ni P2 Ru S2'
_chemical_formula_weight         822.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-24
_audit_creation_method           SHELXL-97
_audit_update_record
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? 
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_cell_angle_alpha                90.00
_cell_angle_beta                 93.216(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.946(3)
_cell_length_b                   10.525(2)
_cell_length_c                   24.884(5)
_cell_measurement_reflns_used    1792
_cell_measurement_temperature    181(2)
_cell_measurement_theta_max      23.01
_cell_measurement_theta_min      2.19
_cell_volume                     3908.3(13)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.2-0 (Bruker, 2013)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
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_computing_publication_material
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
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XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      181.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1629
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_theta_full        25.54
_diffrn_reflns_theta_max         25.54
_diffrn_reflns_theta_min         1.36
_diffrn_source                   'I\ms microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.6317
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1534 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.6326.
The \l/2 correction factor is 0.0015.
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_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_preparation
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The data crystal was mounted using oil (Parantone-N) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 3 1) scattering 
planes roughly normal to the spindle axis. 
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_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         7263
_refine_ls_number_restraints     373
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1429
_reflns_number_gt                4731
_reflns_number_total             7263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4006824_si_002.cif
_cod_data_source_block           fm34c_0m
_cod_database_code               4081855
_olex2_refinement_description
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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
 C30-C31 \\sim C30-C35 \\sim C30A-C31A \\sim C30A-C35A
 with sigma of 0.01
 C31-C32 \\sim C34-C35 \\sim C31A-C32A \\sim C34A-C35A
 with sigma of 0.01
 C33-C32 \\sim C33-C34 \\sim C33A-C32A \\sim C33A-C34A
 with sigma of 0.01
 C33-C39 \\sim C33A-C39A
 with sigma of 0.01
 C34-C39 \\sim C32-C39 \\sim C34A-C39A \\sim C32A-C39A
 with sigma of 0.02
 C30-C36 \\sim C30A-C36A
 with sigma of 0.01
 C36-C35 \\sim C36-C31 \\sim C36A-C35A \\sim C36A-C31A
 with sigma of 0.02
 C36-C37 \\sim C36-C38 \\sim C36A-C37A \\sim C36A-C38A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C34A \\sim C31 \\sim C35A \\sim C32 \\sim C30A \\sim C33 
\\sim C31A \\sim C34 \\sim C35 \\sim C32A \\sim C33A 
\\sim C30: within 1.7A with sigma of 0.02 and sigma for 
terminal atoms of 0.04
C36A \\sim C38A \\sim C39 \\sim C37A \\sim C39A \\sim C37 
\\sim C36 \\sim C38: within 1.7A with sigma of 0.01 and 
sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C35A) 
\\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C35) 
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C32) 
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32A) 
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34A) 
\\sim Ueq, Uanis(C33A) \\sim Ueq: with sigma of 0.01 
and sigma for terminal atoms of 0.02
Uanis(C36A) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C39) 
\\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C36) 
\\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C37) 
\\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(C34A)=
 Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37D)=
 Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39A)=
 Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(C30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(C34)=Sof(H34)=
 Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C15(H15), C1(H1), C7(H7), C36(H36), C36A(H36A)
5.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C14(H14A,H14B), C13(H13A,
 H13B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C20(H20A,H20B), C19(H19A,H19B), C18(H18A,H18B), C17(H17A,H17B),
  C16(H16A,H16B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,
 H6B), C12(H12A,H12B), C11(H11A,H11B), C10(H10A,H10B), C9(H9A,H9B), C8(H8A,H8B)
5.c Me refined with riding coordinates:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C37A(H37D,H37E,H37F), C38A(H38D,
 H38E,H38F)
5.d Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C34(H34), C35(H35), C31A(H31A), C32A(H32A), C34A(H34A),
 C35A(H35A)
5.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F)
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