Synthesis and Structure of Distanna and Tristanna Ansa Half-Sandwich Complexes of Ruthenium and Nickel
Holger Braunschweig; Rainer Dörfler; Kai Hammond; Thomas Kramer; Jan Mies; Krzysztof Radacki; Marius Schäfer; Inorganic Chemistry 51 (2012) 1225–1227; doi:10.1021/ic202512y

data_4328284
_publ_contact_author_address
; Institut fuer Anorganische Chemie
Universitaet Wuerzburg
Am Hubland
97074 Wuerzburg, Germany
;
_publ_contact_author_email       H.Braunschweig@mail.uni-wuerzburg.de
_publ_contact_author_fax         +49-931-3184623
_publ_contact_author_name        'Prof. Dr. Holger Braunschweig'
_publ_contact_author_phone       +49-931-3185260
_publ_section_title
;
 Synthesis and Structure of Distanna and Tristanna Ansa Half-Sandwich
 Complexes of Ruthenium and Nickel
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1225
_journal_page_last               1227
_journal_paper_doi               10.1021/ic202512y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C30 H58 Ni O Sn3'
_chemical_formula_sum            'C30 H58 Ni O Sn3'
_chemical_formula_weight         849.54
_chemical_name_common
;
?
;
_chemical_name_systematic
; 
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.351(2)
_cell_angle_beta                 107.504(2)
_cell_angle_gamma                93.868(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8423(6)
_cell_length_b                   11.1459(6)
_cell_length_c                   17.0318(9)
_cell_measurement_reflns_used    8160
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.54
_cell_volume                     1898.22(18)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7439
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    2.456
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       needle
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The crystalisation was done from hexene solution. It was however not possible
to find properly defined hexene molecule in solvent void.
;
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.5689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0593
_reflns_number_gt                6907
_reflns_number_total             7439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202512y_si_001_4.cif
_cod_data_source_block           4
_cod_database_code               4328284