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_7037188
_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         'C60 H51 Cl O2 P4 Ru, C H2 Cl2'
_chemical_formula_sum            'C61 H53 Cl3 O2 P4 Ru'
_chemical_formula_weight         1149.33
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-02
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Mar 21 2013 11:16:32, GUI svn.r4446)
;
_audit_update_record
;
2015-09-21 deposited with the CCDC.
2015-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                103.3270(10)
_cell_angle_beta                 91.8920(10)
_cell_angle_gamma                104.7960(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8804(4)
_cell_length_b                   11.4875(4)
_cell_length_c                   24.2218(9)
_cell_measurement_reflns_used    8190
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.98
_cell_measurement_theta_min      2.21
_cell_volume                     2834.62(18)
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            53960
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         31.02
_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    0.572
_exptl_absorpt_correction_T_max  0.9011
_exptl_absorpt_correction_T_min  0.6058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0441 before and 0.0282 after correction.
The Ratio of minimum to maximum transmission is 0.6723.
The \l/2 correction factor is 0.0015.
;
_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    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.062
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         15073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                11861
_reflns_number_total             15073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03844h2.cif
_cod_data_source_block           13srv107
_cod_depositor_comments
'Adding full bibliography for 7037188--7037194.cif.'
_cod_database_code               7037188
_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. Others
 Fixed Sof: O1(0.5) O1A(0.5) O2(0.5) O2A(0.5) C3(0.5) C4(0.5) H4(0.5) C5(0.5)
 H5(0.5) C6(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) C3A(0.5) C8A(0.5) H8A(0.5)
 C7A(0.5) H7A(0.5) C6A(0.5) C5A(0.5) H5A(0.5) C4A(0.5) H4A(0.5) C9(0.5)
 C9A(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C10A(0.5) H10D(0.5) H10E(0.5)
 H10F(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C1S(H1SA,H1SB)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C8A(H8A), C7A(H7A), C5A(H5A), C4A(H4A),
 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), C61(H61), C62(H62), C63(H63),
  C64(H64), C65(H65), 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)
3.c Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8), C3A(C8A,C7A,C6A,C5A,C4A)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F)
;