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_4085527
_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         'C96 H74 P4 Ru2, C H2 Cl2'
_chemical_formula_sum            'C97 H76 Cl2 P4 Ru2'
_chemical_formula_weight         1638.50
_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             2012-10-01
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled 2012.08.15 svn.r2450, GUI svn.r4314)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.678(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.693(7)
_cell_length_b                   11.384(4)
_cell_length_c                   21.646(9)
_cell_measurement_reflns_used    7378
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      2.53
_cell_volume                     4066(3)
_computing_cell_refinement       'Rigaku CrystalClear (Rigaku Inc., 2008)'
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku Saturn 724+ CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           'synchrotron '
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20671
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         2.04
_diffrn_source
;
undulator, Beamline I19, Diamond Light Source, RAL
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1445 before and 0.0893 after correction.
The Ratio of minimum to maximum transmission is 0.6559.
The \l/2 correction factor is Not present.
;
_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    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.001
_refine_diff_density_max         1.179
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0800
_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^)+(0.1500P)^2^+8.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2575
_reflns_number_gt                3957
_reflns_number_total             6114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501186c_si_002.cif
_cod_data_source_block           5_d12srv194
_cod_depositor_comments
'Adding full bibliography for 4085524--4085528.cif.'
_cod_database_code               4085527