Sandwich and half-sandwich metal complexes derived from cross-conjugated 3-methylene-penta-1,4-diynes.
Vincent, Kevin B.; Gluyas, Josef B. G.; Zeng, Qiang; Yufit, Dmitry S.; Howard, Judith A. K.; Hartl, František; Low, Paul J.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5522–5531; doi:10.1039/c6dt04470k

data_7041534
_publ_section_title
;
 Sandwich and half-sandwich metal complexes derived from cross-conjugated
 3-methylene-penta-1,4-diynes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5522
_journal_page_last               5531
_journal_paper_doi               10.1039/c6dt04470k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C59 H47 P2 Ru, 2(C H2 Cl2), F6 P'
_chemical_formula_sum            'C61 H51 Cl4 F6 P3 Ru'
_chemical_formula_weight         1233.80
_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             2013-05-30
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2016-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.0958(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.10121(19)
_cell_length_b                   31.5936(4)
_cell_length_c                   14.8655(2)
_cell_measurement_reflns_used    23955
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.5700
_cell_measurement_theta_min      2.7540
_cell_volume                     5535.58(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9413
_diffrn_measurement_details
;
  1 omega  -63.00   21.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.1092   77.0000  120.0000 84

  2 omega  -98.00   45.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.1092    0.0000 -120.0000 143

  3 omega  -78.00  -23.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.1092  -57.0000    0.0000 55

  4 omega  -92.00  -45.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.1092   19.0000 -180.0000 47

  5 omega    4.00   74.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7342 -100.0000  -30.0000 70

  6 omega    4.00   68.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7342 -100.0000 -150.0000 64

  7 omega   33.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       30.7342   57.0000  -90.0000 38

  8 omega  -54.00   40.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.1092   57.0000  -90.0000 94

  9 omega -103.00    3.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.1092  -77.0000 -120.0000 106

 10 omega -103.00  -38.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.1092  -77.0000    0.0000 65

 11 omega -101.00   -6.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.1092  -57.0000  120.0000 95
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      0.0001527000
_diffrn_orient_matrix_UB_12      -0.0186623000
_diffrn_orient_matrix_UB_13      0.0265429000
_diffrn_orient_matrix_UB_21      -0.0579954000
_diffrn_orient_matrix_UB_22      0.0033087000
_diffrn_orient_matrix_UB_23      -0.0000168000
_diffrn_orient_matrix_UB_31      -0.0160686000
_diffrn_orient_matrix_UB_32      -0.0120307000
_diffrn_orient_matrix_UB_33      -0.0411707000
_diffrn_radiation_collimation    monochromator
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_xray_symbol    Mo
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            92790
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.58
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.5378
_exptl_crystal_size_mid          0.2673
_exptl_crystal_size_min          0.1265
_refine_diff_density_max         1.447
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         14013
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0300P)^2^+11.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                11904
_reflns_number_total             14013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt04470k1.cif
_cod_data_source_block           4a_13srv163
_cod_depositor_comments
'Adding full bibliography for 7041533--7041535.cif.'
_cod_original_cell_volume        5535.60(13)
_cod_database_code               7041534
_chemical_oxdiff_formula         'C61 H51 P3 F6 Ru1 Cl4'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl4-C2S \\sim Cl5-C2S
 with sigma of 0.005
3. Others
 Fixed Sof: Cl4(0.7) Cl5(0.3)
4.a Riding coordinates:
 C2S(H2SA)
4.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), 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), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96)
4.d :
 C5(H5)
;