Cationic Terminal Gallylene Complexes by Halide Abstraction: Coordination Chemistry of a Valence Isoelectronic Analogue of CO and N2
Natalie D. Coombs; Dragoslav Vidovic; Joanna K. Day; Amber L. Thompson; Delphine D. Le Pevelen; Andreas Stasch; William Clegg; Luca Russo; Louise Male; Michael B. Hursthouse; David J. Willock; Simon Aldridge; Journal of the American Chemical Society 130 (2008) 16111–16124; doi:10.1021/ja806655f

data_4108744
_publ_contact_author             'Simon Aldridge'
_publ_contact_author_email       Simon.Aldridge@chem.ox.ac.uk
_publ_section_title
;
 Cationic Terminal Gallylene Complexes by Halide Abstraction: Coordination
 Chemistry of a Valence Isoelectronic Analogue of CO and N2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16111
_journal_page_last               16124
_journal_paper_doi               10.1021/ja806655f
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C36 H39 Cl Fe P2 + C32 H12 B F24 -'
_chemical_formula_sum            'C68 H51 B Cl F24 Fe P2'
_chemical_formula_weight         1488.14
_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                 92.724(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.928(5)
_cell_length_b                   25.697(8)
_cell_length_c                   17.157(5)
_cell_measurement_reflns_used    953
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.11
_cell_measurement_theta_min      2.37
_cell_volume                     6574(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6911
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35824
_diffrn_reflns_theta_full        21.33
_diffrn_reflns_theta_max         21.33
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       plate
_exptl_crystal_F_000             3012
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0024(4)
_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   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         8010
_refine_ls_number_restraints     528
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+13.9616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1703
_reflns_number_gt                5727
_reflns_number_total             8010
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja806655f_si_001_09.cif
_cod_data_source_block           11
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4108744