Coordinating Tectons: Bimetallic Complexes from Bipyridyl Terminated Group 8 Alkynyl Complexes
Koutsantonis, George A.; Low, Paul J.; Mackenzie, Campbell F. R.; Skelton, Brian W.; Yufit, Dmitry S.; Organometallics 33 (2014) 4911–; doi:10.1021/om500172r

data_4084208
_publ_section_title
;
 Coordinating Tectons: Bimetallic Complexes from Bipyridyl Terminated
 Group 8 Alkynyl Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4911
_journal_paper_doi               10.1021/om500172r
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C58 H47 Cl N2 P2 Ru2, 2(C H2 Cl2)'
_chemical_formula_sum            'C60 H51 Cl5 N2 P2 Ru2'
_chemical_formula_weight         1241.36
_chemical_name_systematic
;
 ? 
;
_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             2012-11-01
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Oct 26 2012 17:06:22, GUI svn.r4371)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.6880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6207(6)
_cell_length_b                   17.2466(6)
_cell_length_c                   21.6952(8)
_cell_measurement_reflns_used    8588
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.19
_cell_volume                     5653.8(4)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
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_publication_material
;
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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1153
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            106732
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         31.05
_diffrn_reflns_theta_min         0.97
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0632 before and 0.0447 after correction.
The Ratio of minimum to maximum transmission is 0.6712.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear reddish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.943
_refine_diff_density_min         -2.016
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         12966
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0550P)^2^+6.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                8883
_reflns_number_total             12966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500172r_si_001.cif
_cod_data_source_block           6_12srv211
_cod_database_code               4084208
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H46 of C46, H65 of C65, H56 of C56, H43 of C43, H62 of C62, H52 of C52, H53
  of C53, H45 of C45, H5 of C5, H4 of C4, H3 of C3, H82 of C82, {H2SA,H2SB} of
  C2S, {H1SA,H1SB} of C1S, H86 of C86, H63 of C63, H85 of C85, H84 of C84, H35
  of C35, H73 of C73, H74 of C74, H54 of C54, H66 of C66, H72 of C72, H42 of
  C42, H44 of C44, H83 of C83, H55 of C55, H75 of C75, H22 of C22, H64 of C64,
  H34 of C34, H36 of C36, H10 of C10, H9 of C9, H8 of C8, H7 of C7, H6 of C6,
  H33 of C33, H21 of C21, H20 of C20, H19 of C19, H32 of C32, H76 of C76, H16
  of C16, H15 of C15, H13 of C13, H12 of C12, H11 of C11
2. Restrained distances
 Cl5A-C2S \\sim Cl5B-C2S
 with sigma of 0.002
3. Others
 Fixed Sof: Cl5A(0.6) Cl5B(0.4)
4.a Riding coordinates:
 C2S(H2SA,H2SB)
4.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73),
 C74(H74), C75(H75), C76(H76), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
;