Crystal Structure and Computational Investigation of an Analogue of Grubbs' Second Generation Catalyst with a Fluorous Phosphine
Robert Tuba; Edward N. Brothers; Joseph H. Reibenspies; Hassan S. Bazzi; John A. Gladysz; Inorganic Chemistry 51 (2012) 9943–9949; doi:10.1021/ic301434g

data_4330394
_publ_section_title
;
 Crystal Structure and Computational Investigation of an Analogue of
 Grubbs' Second Generation Catalyst with a Fluorous Phosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9943
_journal_page_last               9949
_journal_paper_doi               10.1021/ic301434g
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C58 H44 Cl2 F51 N2 P Ru'
_chemical_formula_weight         1940.89
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.797(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5824(14)
_cell_length_b                   13.5779(14)
_cell_length_c                   40.186(4)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      44.38
_cell_measurement_theta_min      3.31
_cell_volume                     7323.9(13)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'MWPC area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1063
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            158644
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    4.197
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.6135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'pale_red  '
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       plate
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.00101(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1525
_refine_ls_number_reflns         10815
_refine_ls_number_restraints     1905
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.002
_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          0.1384
_refine_ls_wR_factor_ref         0.1460
_reflns_number_gt                7056
_reflns_number_total             10815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301434g_si_002.cif
_cod_data_source_block           jgrt
_cod_original_cell_volume        7324.0(13)
_cod_database_code               4330394