Reactions of alkynes with cis-RuCl2(dppm)2: exploring the interplay of vinylidene, alkynyl and η(3)-butenynyl complexes.
Eaves, Samantha G.; Yufit, Dmitry S.; Skelton, Brian W.; Lynam, Jason M.; Low, Paul J.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 21016–21024; doi:10.1039/c5dt03844h

data_7037192
_publ_section_title
;
 Reactions of alkynes with cis-RuCl2(dppm)2: exploring the interplay of
 vinylidene, alkynyl and \h(3)-butenynyl complexes.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              21016
_journal_page_last               21024
_journal_paper_doi               10.1039/c5dt03844h
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C59 H52 Cl O P4 Ru, C H2 Cl2'
_chemical_formula_sum            'C60 H54 Cl3 O P4 Ru'
_chemical_formula_weight         1122.33
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-11
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr  9 2013 14:06:00, GUI svn.r4452)
;
_audit_update_record
;
2015-09-21 deposited with the CCDC.
2015-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.6030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5876(3)
_cell_length_b                   22.2227(7)
_cell_length_c                   12.7177(4)
_cell_measurement_reflns_used    8404
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.35
_cell_volume                     2582.78(14)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_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            31889
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.68
_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    0.625
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0439 before and 0.0293 after correction.
The Ratio of minimum to maximum transmission is 0.3151.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dull light yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.970
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         13673
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1626
_reflns_number_gt                11817
_reflns_number_total             13673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03844h2.cif
_cod_data_source_block           2f_13srv112
_cod_depositor_comments
'Adding full bibliography for 7037188--7037194.cif.'
_cod_database_code               7037192
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Ru1-Cl1 \\sim Ru1-Cl1A
 with sigma of 0.005
 Cl3-C1S \\sim Cl2-C1S
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(C3A) = Uiso(C4A) = Uiso(C5A) = Uiso(C6A) = Uiso(C7A) = Uiso(C8A)
Uiso(Cl2A) = Uiso(C1C) = Uiso(Cl3A)
4. Others
 Fixed Sof: Cl1(0.75) Cl1A(0.25) O1(0.75) O1A(0.25) C1(0.75) C1A(0.25)
 C2(0.75) C2A(0.25) C3(0.75) C3A(0.25) C4(0.75) H4(0.75) C4A(0.25) H4A(0.25)
 C5(0.75) H5(0.75) C5A(0.25) H5A(0.25) C6(0.75) C6A(0.25) C7(0.75) H7(0.75)
 C7A(0.25) H7A(0.25) C8(0.75) H8(0.75) C8A(0.25) H8A(0.25) C9(0.75) H9A(0.75)
 H9B(0.75) H9C(0.75) C9A(0.25) H9AA(0.25) H9AB(0.25) H9AC(0.25) Cl2(0.75)
 Cl3(0.75) C1S(0.75) H1SA(0.75) H1SB(0.75) Cl2A(0.25) Cl3A(0.25) C1C(0.25)
 H1CA(0.25) H1CB(0.25)
5.a Riding coordinates:
 C9A(H9AA,H9AB,H9AC)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C56(H56A,H56B), C1S(H1SA,H1SB), C1C(H1CA,H1CB)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C4A(H4A), C5(H5), C5A(H5A), C7(H7), C7A(H7A), C8(H8), C8A(H8A),
 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), 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), C92(H92), C93(H93), C94(H94), C95(H95),
  C96(H96)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;