Rational Synthesis and Reversible Metal−Metal Bond Scission of Heterobimetallic Xenophilic Complexes Containing an Unsupported, Polar Metal−Metal Bond, TpiPr2M−Co(CO)3L (M = Ni, Co, Fe, Mn; L = CO, PPh3)
Uehara, Kazuhiro; Hikichi, Shiro; Akita, Munetaka; Organometallics 20 (2001) 5002–; doi:10.1021/om010651j

data_4089316
_publ_section_title
;
 Rational Synthesis and Reversible Metal&#x2212;Metal Bond Scission of
 Heterobimetallic Xenophilic Complexes Containing an Unsupported, Polar
 Metal&#x2212;Metal Bond, TpiPr2M&#x2212;Co(CO)3L (M = Ni, Co, Fe, Mn; L =
 CO, PPh3)
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5002
_journal_paper_doi               10.1021/om010651j
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C25 H33 B Br3 Co N6 Ni O4'
_chemical_formula_weight         849.75
_chemical_name_common            'compound 1'Ni_hexane'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 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                 104.545(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8178(14)
_cell_length_b                   13.9755(10)
_cell_length_c                   11.3967(8)
_cell_measurement_temperature    213(2)
_cell_volume                     3363.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7408
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    4.655
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1688
_refine_diff_density_max         0.408
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.781
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         7408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.781
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                4688
_reflns_number_total             7408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010651j.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
 Corrected the values of the '_diffrn_radiation_type' and
 '_refine_ls_weighting_details' data items by replacing a
 sequence of malformed symbols with the backslash symbol ('\')
 after consulting the original publication.

 Antanas Vaitkus,
 2019-12-11
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_cod_database_code               4089316