Taking Advantage of Hg−C Bonds: Synthesis of the First Homoleptic Bis-β-diketiminate Complex Bound through the γ-Carbons
Ferro, Lorenzo; Coles, Martyn P.; Day, Iain J.; Fulton, J. Robin; Organometallics 29 (2010) 2911–; doi:10.1021/om100167e

data_4065861
_publ_section_title
;
 Taking Advantage of Hg&#x2212;C Bonds: Synthesis of the First Homoleptic
 Bis-\b-diketiminate Complex Bound through the \g-Carbons
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2911
_journal_paper_doi               10.1021/om100167e
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H82 Hg1 N4, 0.33(C H2 Cl2)'
_chemical_formula_sum            'C58.33 H82.66 Cl0.66 Hg N4'
_chemical_formula_weight         1064.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2010-05-25T08:56:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   33.4216(10)
_cell_length_b                   33.4216(10)
_cell_length_c                   12.6432(3)
_cell_measurement_reflns_used    12307
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     12230.4(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.286678E-1
_diffrn_orient_matrix_UB_12      0.178552E-1
_diffrn_orient_matrix_UB_13      0.431513E-1
_diffrn_orient_matrix_UB_21      -0.191438E-1
_diffrn_orient_matrix_UB_22      -0.8692E-3
_diffrn_orient_matrix_UB_23      0.616922E-1
_diffrn_orient_matrix_UB_31      -0.23109E-2
_diffrn_orient_matrix_UB_32      -0.295653E-1
_diffrn_orient_matrix_UB_33      0.242464E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.047
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17578
_diffrn_reflns_theta_full        26.72
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.903
_exptl_absorpt_correction_T_max  0.4145
_exptl_absorpt_correction_T_min  0.3498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.37
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5220
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+29.9175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                5104
_reflns_number_total             5739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100167e_si_002.cif
_cod_data_source_block           feb310b
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4065861