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_4108739
_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         'C45 H50 Fe1 Ga1 I1 P2, 0.75(C4 H10 O)'
_chemical_formula_sum            'C48 H57.5 Fe Ga I O0.75 P2'
_chemical_formula_weight         960.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-08-05
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 106.2212(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5305(4)
_cell_length_b                   15.2373(4)
_cell_length_c                   21.0196(7)
_cell_measurement_reflns_used    31856
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     4468.6(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.109
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49199
_diffrn_reflns_theta_full        26.178
_diffrn_reflns_theta_max         26.712
_diffrn_reflns_theta_min         2.858
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.723
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       plate
_exptl_crystal_F_000             1966.000
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.54
_refine_diff_density_min         -1.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6665
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.000716
_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: 
 1.25 -0.839 0.719 -0.314 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0857
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0736
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6665
_reflns_number_total             9418
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.97
_oxford_diffrn_Wilson_scale      44.14
_oxford_refine_ls_r_factor_ref   0.0834
_oxford_refine_ls_scale          0.1578(3)
_oxford_reflns_number_all        9400
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title SA-0608
_cod_data_source_file            ja806655f_si_001_04.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C48 H57.50 Fe1 Ga1 I1 O0.75 P2'
_cod_database_code               4108739