Heterometallic Multiple Bonding: Delocalized Three-Center σ and π Bonding in Chains of 4d and 5d Transition Metals.
Brogden, David W.; Berry, John F.; Inorganic chemistry 53 (2014) 11354–11356; doi:10.1021/ic5024218

data_4341285
_publ_section_title
;
 Heterometallic Multiple Bonding: Delocalized Three-Center \s and \p
 Bonding in Chains of 4d and 5d Transition Metals.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11354
_journal_page_last               11356
_journal_paper_doi               10.1021/ic5024218
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'2(C40 H32 Cl1.9 N12 Ru0.96 W1.92), 0.08(Cl2 Ru W2), 4(C H2 Cl2)'
_chemical_formula_sum            'C84 H72 Cl11.98 N24 Ru2 W4'
_chemical_formula_weight         2779.90
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.5734(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7217(5)
_cell_length_b                   29.7782(8)
_cell_length_c                   16.7192(4)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      2.19
_cell_volume                     8929.5(4)
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  Gromit
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            232439
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.25
_diffrn_reflns_theta_min         1.14
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.881
_exptl_absorpt_correction_T_max  0.8304
_exptl_absorpt_correction_T_min  0.4352
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2010) was used for absorption correction.
wR2(int) was 0.1049 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.5241.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5327
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.053
_refine_diff_density_max         3.568
_refine_diff_density_min         -3.108
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         24193
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+92.3151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                19636
_reflns_number_total             24193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5024218_si_003.cif
_cod_data_source_block           berry528
_cod_depositor_comments
'Adding full bibliography for 4341284--4341285.cif.'
_cod_database_code               4341285
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{W2, W2A}
3. Uiso/Uaniso restraints and constraints
Uanis(W1) = Uanis(Ru1A)
Uanis(W2) = Uanis(W2A)
Uanis(W1A) = Uanis(Ru1)
Uanis(W3A) = Uanis(Ru2)
Uanis(W4) = Uanis(W4A)
Uanis(Ru2A) = Uanis(W3)
4. Same fragment restrains
{Ru1A, W1A, W2A, Cl2A, Cl1A}
as
{Ru1, W1, W2, Cl1, Cl2}
{Ru2A, W3A, W4A, Cl4A, Cl3A}
as
{Ru2, W3, W4, Cl3, Cl4}
5. Others
 Sof(Cl13)=Sof(Cl14)=Sof(C86)=Sof(H86A)=Sof(H86B)=1-FVAR(1)
 Sof(Cl11)=Sof(Cl12)=Sof(C84)=Sof(H84A)=Sof(H84B)=FVAR(1)
 Sof(Cl15)=Sof(Cl16)=Sof(C85)=Sof(H85A)=Sof(H85B)=1-FVAR(2)
 Sof(Cl5)=Sof(Cl6)=Sof(C81)=Sof(H81A)=Sof(H81B)=FVAR(2)
 Sof(Ru1A)=Sof(W1A)=Sof(W2A)=Sof(Cl2A)=Sof(Cl1A)=1-FVAR(3)
 Sof(Ru1)=Sof(W1)=Sof(W2)=Sof(Cl2)=FVAR(3)
 Sof(Ru2A)=Sof(W3A)=Sof(W4A)=Sof(Cl4A)=Sof(Cl3A)=1-FVAR(4)
 Sof(Ru2)=Sof(W3)=Sof(W4)=Sof(Cl3)=Sof(Cl4)=FVAR(4)
6.a Free rotating group:
 Cl13(Cl14,C86,C82,Cl8), Cl15(Cl16,C85,Cl9,Cl10,C83,Cl5,Cl6,C81,Cl7)
6.b Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B), C86(H86A,H86B), C82(H82A,H82B), C85(H85A,H85B), C83(H83A,
 H83B), C81(H81A,H81B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), C47(H47), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C57(H57), C58(H58), C59(H59),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C67(H67), C68(H68),
 C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C77(H77), C78(H78),
  C79(H79), C80(H80)
;
_olex2_submission_special_instructions 'No special instructions were received'