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_7037193
_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_formula_moiety         'C70 H58 O4 P4 Ru, C H Cl3'
_chemical_formula_sum            'C71 H59 Cl3 O4 P4 Ru'
_chemical_formula_weight         1307.48
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-20
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Mar 13 2013 19:31:35, GUI svn.r4414)
;
_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                 104.388(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7726(15)
_cell_length_b                   13.9939(12)
_cell_length_c                   25.218(2)
_cell_measurement_reflns_used    3137
_cell_measurement_temperature    120
_cell_measurement_theta_max      24.43
_cell_measurement_theta_min      2.17
_cell_volume                     6075.2(9)
_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  0.2025
_diffrn_reflns_av_unetI/netI     0.1540
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34789
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.67
_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    0.546
_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    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.973
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7324
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1935
_reflns_number_gt                3694
_reflns_number_total             7324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03844h2.cif
_cod_data_source_block           3b_13srv102
_cod_depositor_comments
'Adding full bibliography for 7037188--7037194.cif.'
_cod_original_cell_volume        6075.1(9)
_cod_database_code               7037193
_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
 Cl4-C1S \\sim Cl3-C1S \\sim Cl5-C1S \\sim Cl1-C1S \\sim Cl2-C1S
 with sigma of 0.01
3. Others
 Fixed Sof: Cl1(0.5) Cl2(0.25) Cl3(0.25) Cl4(0.25) Cl5(0.25) C1S(0.5) H1S(0.5)
4.a Everything fixed:
 H1S
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), 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)
4.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;