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_4084209
_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         'C56 H42 Cl N2 O3 P2 Re Ru, 0.25(C H2 Cl2)'
_chemical_formula_sum            'C56.25 H42.5 Cl1.5 N2 O3 P2 Re Ru'
_chemical_formula_weight         1196.81
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-20
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                79.346(6)
_cell_angle_beta                 88.646(7)
_cell_angle_gamma                82.748(7)
_cell_formula_units_Z            2
_cell_length_a                   11.1754(10)
_cell_length_b                   13.7333(10)
_cell_length_c                   17.7887(14)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.407
_cell_measurement_theta_min      2.986
_cell_volume                     2661.6(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Rigaku CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'Bruker APEX2'
_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      100.0(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Rigaku Saturn 724+ CCD area detector'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           'synchrotron '
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23736
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.13
_diffrn_source
'undulator, Beamline I19, Diamond Light Source, RAL'
_exptl_absorpt_coefficient_mu    2.504
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1515 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.6742.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1185
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.001
_refine_diff_density_max         2.448
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         10847
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0860P)^2^+4.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1466
_reflns_number_gt                8452
_reflns_number_total             10847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500172r_si_001.cif
_cod_data_source_block           7_12srv212
_cod_original_formula_sum        'C56.25 H42.50 Cl1.50 N2 O3 P2 Re Ru'
_cod_database_code               4084209
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H12 of C12, H11 of C11, H10 of C10, H35 of C35, H34 of C34, H23 of C23, H22
  of C22, H52 of C52, H46 of C46, H53 of C53, H33 of C33, H32 of C32, H18 of
  C18, H17 of C17, H25A of C25A, H26A of C26A, H22A of C22A, H23A of C23A, H24A
  of C24A, H43 of C43, H54 of C54, H9 of C9, H8 of C8, H45 of C45, H26 of C26,
  H25 of C25, H24 of C24, H74 of C74, H73 of C73, H72 of C72, H66 of C66, H65
  of C65, H64 of C64, H63 of C63, H62 of C62, H56 of C56, H55 of C55, H5 of C5,
  H4 of C4, H16 of C16, {H1SA,H1SB} of C1S, H76 of C76, H75 of C75, H42 of C42,
  H20 of C20, H19 of C19, H44 of C44, H36 of C36
2. Restrained distances
 O1-C15
 1.15 with sigma of 0.005
 Cl2-C1S = Cl3-C1S
 1.8 with sigma of 0.02
 Cl2-C1S \\sim Cl3-C1S
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C21(0.5) C21A(0.5) C26A(0.5) H26A(0.5) C25A(0.5) H25A(0.5)
 C24A(0.5) H24A(0.5) C23A(0.5) H23A(0.5) C22A(0.5) H22A(0.5) C22(0.5) H22(0.5)
 C23(0.5) H23(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5)
 Cl2(0.25) Cl3(0.25) C1S(0.25) H1SA(0.25) H1SB(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C26A(H26A), C25A(H25A), C24A(H24A),
 C23A(H23A), C22A(H22A), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 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)
5.c Fitted hexagon refined as free rotating group:
 C21A(C26A,C25A,C24A,C23A,C22A)
;