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_4108743
_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         'C32 H12 B1 F24, C24 H30 Fe2 I1 O4, C6 H5 F1'
_chemical_formula_sum            'C62 H47 B F25 Fe2 I O4'
_chemical_formula_weight         1580.41
_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
_audit_creation_date             08-02-04
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 93.6797(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6058(2)
_cell_length_b                   16.3640(2)
_cell_length_c                   21.0354(2)
_cell_measurement_reflns_used    14875
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     6391.35(12)
_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 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.068
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            83503
_diffrn_reflns_theta_full        26.945
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         5.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_red
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       plate
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.86
_refine_diff_density_min         -1.58
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         10967
_refine_ls_number_restraints     116
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.001341
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.955 0.638 0.529 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0922
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0718
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                10967
_reflns_number_total             14560
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.05
_oxford_diffrn_Wilson_scale      37.81
_oxford_refine_ls_r_factor_ref   0.0641
_oxford_refine_ls_scale          0.1757(3)
_oxford_reflns_number_all        14558
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 5682
_cod_data_source_file            ja806655f_si_001_08.cif
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4108743