Pentamethylcyclopentadienyl Half-Sandwich Diazoalkane Complexes of Ruthenium: Preparation and Reactivity.
Albertin, Gabriele; Antoniutti, Stefano; Bortoluzzi, Marco; Botter, Alessandra; Castro, Jesús; Inorganic chemistry 55 (2016) 5592–5602; doi:10.1021/acs.inorgchem.6b00671

data_4347832
_publ_section_title
;
 Pentamethylcyclopentadienyl Half-Sandwich Diazoalkane Complexes of
 Ruthenium: Preparation and Reactivity.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5592
_journal_page_last               5602
_journal_paper_doi               10.1021/acs.inorgchem.6b00671
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C59 H73 B N2 O6 P2 Ru'
_chemical_formula_weight         1080.01
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           Monoclinic'
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.161(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7683(10)
_cell_length_b                   21.0912(18)
_cell_length_c                   19.7024(14)
_cell_measurement_reflns_used    2185
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.54
_cell_measurement_theta_min      31.12
_cell_volume                     5706.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker CCD Smart 6000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec Quazar MX multilayer optics'
_diffrn_radiation_source         'Incoatec I\muS microsource'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66279
_diffrn_reflns_theta_full        68.39
_diffrn_reflns_theta_max         68.39
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    3.142
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         10365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+1.0289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                7666
_reflns_number_total             10365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00671_si_002.cif
_cod_data_source_block           2c_md
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4347832