Syntheses and Structures of Buta-1,3-Diynyl Complexes from “on Complex” Cross-Coupling Reactions
Oerthel, Marie-Christine; Yufit, Dmitry S.; Fox, Mark A.; Bryce, Martin R.; Low, Paul J.; Organometallics 34 (2015) 2395–; doi:10.1021/om501186c

data_4085525
_publ_section_title
;
 Syntheses and Structures of Buta-1,3-Diynyl Complexes from &#x201C;on
 Complex&#x201D; Cross-Coupling Reactions
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2395
_journal_paper_doi               10.1021/om501186c
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C52 H42 P2 Ru'
_chemical_formula_sum            'C52 H42 P2 Ru'
_chemical_formula_weight         829.87
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-04
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Oct  2 2012 15:53:34, GUI svn.r4355)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.512(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9342(9)
_cell_length_b                   23.3662(17)
_cell_length_c                   13.3100(10)
_cell_measurement_reflns_used    5943
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.23
_cell_volume                     3978.3(5)
_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      120
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0997
_diffrn_reflns_av_unetI/netI     0.0911
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45590
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.74
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           10.0
_diffrn_source_power             0.3
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           30.0
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         9605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                5906
_reflns_number_total             9605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501186c_si_002.cif
_cod_data_source_block           4b_12srv195
_cod_depositor_comments
'Adding full bibliography for 4085524--4085528.cif.'
_cod_database_code               4085525
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H46 of C46, H52 of C52, H25 of C25, H26 of C26, H16 of C16, H74 of C74, H56
  of C56, H62 of C62, H75 of C75, H64 of C64, H55 of C55, H10 of C10, H44 of
  C44, H24 of C24, H35 of C35, H13 of C13, H12 of C12, H43 of C43, H72 of C72,
  H54 of C54, H23 of C23, H36 of C36, H32 of C32, H76 of C76, H63 of C63, H14
  of C14, H53 of C53, H73 of C73, H22 of C22, H65 of C65, H6 of C6, H66 of C66,
  H34 of C34, H42 of C42, H7 of C7, H33 of C33, H9 of C9, H45 of C45, H15 of C15
 At 1.5 times of:
  {H11A,H11B,H11C} of C11
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), 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)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;