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_4108746
_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         'C31 H32 F1 Ga1 I2 O2 P1 Ru1'
_chemical_formula_sum            'C31 H32 F Ga I2 O2 P Ru'
_chemical_formula_weight         911.16
_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
_audit_creation_date             08-07-21
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                73.8264(8)
_cell_angle_beta                 69.7145(7)
_cell_angle_gamma                85.1463(9)
_cell_formula_units_Z            2
_cell_length_a                   10.8243(2)
_cell_length_b                   11.0082(2)
_cell_length_c                   15.2923(3)
_cell_measurement_reflns_used    7015
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1641.36(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28395
_diffrn_reflns_theta_full        26.961
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         5.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.242
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_description       plate
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.18
_refine_diff_density_min         -1.20
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9910
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.000666
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 4.04P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0854
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0854
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                6189
_reflns_number_total             7466
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.12
_oxford_diffrn_Wilson_scale      27.68
_oxford_refine_ls_r_factor_ref   0.0463
_oxford_refine_ls_scale          0.19726(8)
_oxford_reflns_number_all        7466
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 029dvdv08
_cod_data_source_file            ja806655f_si_001_11.cif
_cod_data_source_block           14
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C31 H32 F1 Ga1 I2 O2 P1 Ru1'
_cod_database_code               4108746