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_4347831
_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_moiety         'C22 H47 N2 O6 P2 Ru, C24 H20 B'
_chemical_formula_sum            'C46 H67 B N2 O6 P2 Ru'
_chemical_formula_weight         917.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                86.480(5)
_cell_angle_beta                 77.936(4)
_cell_angle_gamma                84.995(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1749(9)
_cell_length_b                   14.2023(12)
_cell_length_c                   17.2321(13)
_cell_measurement_reflns_used    6640
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      61.10
_cell_measurement_theta_min      2.62
_cell_volume                     2423.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.965
_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  0.1019
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51904
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.100
_diffrn_reflns_theta_min         2.625
_exptl_absorpt_coefficient_mu    3.602
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.3967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1036P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6998
_reflns_number_total             8538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00671_si_003.cif
_cod_data_source_block           7_md
_cod_database_code               4347831
_shelx_estimated_absorpt_t_min   0.648
_shelx_estimated_absorpt_t_max   0.866
_shelxl_version_number           2014/6
_shelx_res_checksum              46418
_shelx_hkl_checksum              25089