Six-Coordinate Alkynyldiphenylphosphine Ruthenium(II) Complexes: Synthesis, Structure, and Catalytic Activity as ROMP Initiators
Bernechea, María; Lugan, Noël; Gil, Belén; Lalinde, Elena; Lavigne, Guy; Organometallics 25 (2006) 684–; doi:10.1021/om050935u

data_4074837
_publ_section_title
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 Six-Coordinate Alkynyldiphenylphosphine Ruthenium(II) Complexes:&#x00A0;
 Synthesis, Structure, and Catalytic Activity as ROMP Initiators
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_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              684
_journal_paper_doi               10.1021/om050935u
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C71 H57 Cl2 P3 Ru, C4 H10 O'
_chemical_formula_sum            'C75 H67 Cl2 O P3 Ru'
_chemical_formula_weight         1249.17
_chemical_name_common            MBN363
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 91.751(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7880(1)
_cell_length_b                   23.1970(3)
_cell_length_c                   23.2680(3)
_cell_measurement_reflns_used    64292
_cell_measurement_temperature    173.0(10)
_cell_volume                     6359.58(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0020678
_diffrn_orient_matrix_UB_12      0.0430504
_diffrn_orient_matrix_UB_13      0.0020008
_diffrn_orient_matrix_UB_21      -0.0838999
_diffrn_orient_matrix_UB_22      0.0007431
_diffrn_orient_matrix_UB_23      0.0051461
_diffrn_orient_matrix_UB_31      0.0126436
_diffrn_orient_matrix_UB_32      -0.0021097
_diffrn_orient_matrix_UB_33      0.0426406
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.069
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            90941
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         15128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+4.6540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                10271
_reflns_number_total             15128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050935usi20051129_063723.cif
_cod_data_source_block           complex13.Et2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4074837