#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:10:14 +0100 (lun 21 de mar de 2016) $
#$Revision: 178551 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/58/4065861.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4065861
loop_
_publ_author_name
'Ferro, Lorenzo'
'Coles, Martyn P.'
'Day, Iain J.'
'Fulton, J. Robin'
_publ_section_title
;
 Taking Advantage of Hg−C Bonds: Synthesis of the First Homoleptic
 Bis-β-diketiminate Complex Bound through the γ-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 κ-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/[σ²(Fo²)+(0.0173P)²+29.9175P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Hg Hg 0.5 0 0 0.02264(6) Uani 1 2 d S
N1 N 0.55599(8) 0.12470(8) 0.07847(17) 0.0236(5) Uani 1 1 d .
N2 N 0.45834(8) 0.05683(8) -0.06945(16) 0.0195(5) Uani 1 1 d .
C1 C 0.56735(9) 0.09935(10) 0.0256(2) 0.0237(6) Uani 1 1 d .
C2 C 0.53506(9) 0.06883(9) -0.0591(2) 0.0225(6) Uani 1 1 d .
H2 H 0.5539 0.0699 -0.1216 0.027 Uiso 1 1 calc R
C3 C 0.50056(10) 0.08226(9) -0.0949(2) 0.0216(6) Uani 1 1 d .
C4 C 0.60995(10) 0.09562(11) 0.0423(2) 0.0335(7) Uani 1 1 d .
H4C H 0.6242 0.1098 0.1101 0.05 Uiso 1 1 calc R
H4B H 0.6319 0.1116 -0.0151 0.05 Uiso 1 1 calc R
H4A H 0.6014 0.063 0.0429 0.05 Uiso 1 1 calc R
C5 C 0.51958(11) 0.12584(11) -0.1601(2) 0.0341(7) Uani 1 1 d .
H5C H 0.5412 0.1523 -0.1172 0.051 Uiso 1 1 calc R
H5B H 0.4941 0.1303 -0.1834 0.051 Uiso 1 1 calc R
H5A H 0.5357 0.1232 -0.222 0.051 Uiso 1 1 calc R
C6 C 0.58427(9) 0.15198(10) 0.1643(2) 0.0250(6) Uani 1 1 d .
C7 C 0.62492(10) 0.19399(11) 0.1459(2) 0.0313(7) Uani 1 1 d .
C8 C 0.65073(11) 0.21861(12) 0.2331(3) 0.0429(9) Uani 1 1 d .
H8 H 0.6786 0.2471 0.2226 0.051 Uiso 1 1 calc R
C9 C 0.63686(12) 0.20266(13) 0.3349(3) 0.0465(9) Uani 1 1 d .
H9 H 0.6557 0.2193 0.3934 0.056 Uiso 1 1 calc R
C10 C 0.59608(11) 0.16296(12) 0.3510(2) 0.0379(8) Uani 1 1 d .
H10 H 0.5863 0.1529 0.4214 0.045 Uiso 1 1 calc R
C11 C 0.56838(10) 0.13675(11) 0.2672(2) 0.0289(7) Uani 1 1 d .
C12 C 0.63957(11) 0.21285(11) 0.0345(3) 0.0374(8) Uani 1 1 d .
H12 H 0.6277 0.1858 -0.0146 0.045 Uiso 1 1 calc R
C13 C 0.61727(15) 0.24105(16) 0.0028(3) 0.0662(12) Uani 1 1 d .
H13C H 0.5836 0.2214 0.0049 0.099 Uiso 1 1 calc R
H13B H 0.6269 0.253 -0.0691 0.099 Uiso 1 1 calc R
H13A H 0.6269 0.2669 0.052 0.099 Uiso 1 1 calc R
C14 C 0.69186(12) 0.24130(13) 0.0195(3) 0.0519(10) Uani 1 1 d .
H14C H 0.7047 0.268 0.0673 0.078 Uiso 1 1 calc R
H14B H 0.6988 0.2521 -0.0538 0.078 Uiso 1 1 calc R
H14A H 0.7057 0.2221 0.0355 0.078 Uiso 1 1 calc R
C15 C 0.52299(11) 0.09240(11) 0.2849(2) 0.0338(7) Uani 1 1 d .
H15 H 0.5028 0.0882 0.2227 0.041 Uiso 1 1 calc R
C16 C 0.49712(13) 0.09391(15) 0.3845(3) 0.0567(11) Uani 1 1 d .
H16C H 0.5164 0.0989 0.447 0.085 Uiso 1 1 calc R
H16B H 0.4681 0.0646 0.3916 0.085 Uiso 1 1 calc R
H16A H 0.4904 0.1192 0.378 0.085 Uiso 1 1 calc R
C17 C 0.52996(13) 0.05088(13) 0.2882(3) 0.0510(9) Uani 1 1 d .
H17C H 0.5432 0.0485 0.221 0.077 Uiso 1 1 calc R
H17B H 0.5001 0.0228 0.2996 0.077 Uiso 1 1 calc R
H17A H 0.551 0.0546 0.3462 0.077 Uiso 1 1 calc R
C18 C 0.42371(9) 0.06796(9) -0.0987(2) 0.0211(6) Uani 1 1 d .
C19 C 0.41830(10) 0.10110(10) -0.0414(2) 0.0246(6) Uani 1 1 d .
C20 C 0.38070(11) 0.10655(11) -0.0663(2) 0.0317(7) Uani 1 1 d .
H20 H 0.3762 0.1283 -0.0276 0.038 Uiso 1 1 calc R
C21 C 0.34978(11) 0.08128(11) -0.1454(2) 0.0349(8) Uani 1 1 d .
H21 H 0.3244 0.0857 -0.1608 0.042 Uiso 1 1 calc R
C22 C 0.35617(10) 0.04963(11) -0.2018(2) 0.0329(7) Uani 1 1 d .
H22 H 0.3352 0.0326 -0.257 0.04 Uiso 1 1 calc R
C23 C 0.39254(10) 0.04201(10) -0.1798(2) 0.0264(7) Uani 1 1 d .
C24 C 0.45151(11) 0.12993(10) 0.0455(2) 0.0288(7) Uani 1 1 d .
H24 H 0.4771 0.1227 0.0474 0.035 Uiso 1 1 calc R
C25 C 0.47288(12) 0.18170(11) 0.0249(3) 0.0417(8) Uani 1 1 d .
H25C H 0.4897 0.1896 -0.0423 0.063 Uiso 1 1 calc R
H25B H 0.4942 0.199 0.0825 0.063 Uiso 1 1 calc R
H25A H 0.4484 0.1896 0.0215 0.063 Uiso 1 1 calc R
C26 C 0.42763(13) 0.11753(12) 0.1532(2) 0.0424(8) Uani 1 1 d .
H26C H 0.4018 0.1235 0.1527 0.064 Uiso 1 1 calc R
H26B H 0.4498 0.1364 0.2082 0.064 Uiso 1 1 calc R
H26A H 0.416 0.0848 0.168 0.064 Uiso 1 1 calc R
C27 C 0.40017(11) 0.00813(10) -0.2439(2) 0.0308(7) Uani 1 1 d .
H27 H 0.4187 -0.0013 -0.199 0.037 Uiso 1 1 calc R
C28 C 0.42878(15) 0.03143(14) -0.3421(3) 0.0576(11) Uani 1 1 d .
H28C H 0.4125 0.0428 -0.3862 0.086 Uiso 1 1 calc R
H28B H 0.4335 0.0091 -0.3823 0.086 Uiso 1 1 calc R
H28A H 0.4588 0.0574 -0.3209 0.086 Uiso 1 1 calc R
C29 C 0.35580(13) -0.03554(13) -0.2729(3) 0.0566(11) Uani 1 1 d .
H29C H 0.3393 -0.0513 -0.2082 0.085 Uiso 1 1 calc R
H29B H 0.3631 -0.056 -0.3137 0.085 Uiso 1 1 calc R
H29A H 0.3363 -0.0275 -0.3155 0.085 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
C2 Hg C2 180.00(10) 10_655
C1 N1 C6 120.0(2) .
C3 N2 C18 122.2(2) .
N1 C1 C2 118.2(2) .
N1 C1 C4 126.1(3) .
C2 C1 C4 115.6(2) .
C1 C2 C3 114.2(2) .
C1 C2 Hg 107.75(18) .
C3 C2 Hg 109.81(18) .
C1 C2 H2 108.3 .
C3 C2 H2 108.3 .
Hg C2 H2 108.3 .
N2 C3 C2 119.0(2) .
N2 C3 C5 125.0(3) .
C2 C3 C5 115.9(2) .
C1 C4 H4C 109.5 .
C1 C4 H4B 109.5 .
H4C C4 H4B 109.5 .
C1 C4 H4A 109.5 .
H4C C4 H4A 109.5 .
H4B C4 H4A 109.5 .
C3 C5 H5C 109.5 .
C3 C5 H5B 109.5 .
H5C C5 H5B 109.5 .
C3 C5 H5A 109.5 .
H5C C5 H5A 109.5 .
H5B C5 H5A 109.5 .
C7 C6 C11 121.3(3) .
C7 C6 N1 121.0(3) .
C11 C6 N1 117.6(3) .
C8 C7 C6 117.8(3) .
C8 C7 C12 121.0(3) .
C6 C7 C12 121.3(3) .
C9 C8 C7 121.5(3) .
C9 C8 H8 119.3 .
C7 C8 H8 119.3 .
C10 C9 C8 119.7(3) .
C10 C9 H9 120.2 .
C8 C9 H9 120.2 .
C9 C10 C11 121.8(3) .
C9 C10 H10 119.1 .
C11 C10 H10 119.1 .
C10 C11 C6 117.8(3) .
C10 C11 C15 121.9(3) .
C6 C11 C15 120.3(3) .
C13 C12 C7 110.2(3) .
C13 C12 C14 110.2(3) .
C7 C12 C14 113.8(3) .
C13 C12 H12 107.5 .
C7 C12 H12 107.5 .
C14 C12 H12 107.5 .
C12 C13 H13C 109.5 .
C12 C13 H13B 109.5 .
H13C C13 H13B 109.5 .
C12 C13 H13A 109.5 .
H13C C13 H13A 109.5 .
H13B C13 H13A 109.5 .
C12 C14 H14C 109.5 .
C12 C14 H14B 109.5 .
H14C C14 H14B 109.5 .
C12 C14 H14A 109.5 .
H14C C14 H14A 109.5 .
H14B C14 H14A 109.5 .
C11 C15 C17 111.2(3) .
C11 C15 C16 113.0(3) .
C17 C15 C16 110.6(3) .
C11 C15 H15 107.2 .
C17 C15 H15 107.2 .
C16 C15 H15 107.2 .
C15 C16 H16C 109.5 .
C15 C16 H16B 109.5 .
H16C C16 H16B 109.5 .
C15 C16 H16A 109.5 .
H16C C16 H16A 109.5 .
H16B C16 H16A 109.5 .
C15 C17 H17C 109.5 .
C15 C17 H17B 109.5 .
H17C C17 H17B 109.5 .
C15 C17 H17A 109.5 .
H17C C17 H17A 109.5 .
H17B C17 H17A 109.5 .
C19 C18 C23 120.8(3) .
C19 C18 N2 120.7(2) .
C23 C18 N2 118.2(2) .
C20 C19 C18 117.7(3) .
C20 C19 C24 120.2(3) .
C18 C19 C24 122.1(3) .
C21 C20 C19 122.1(3) .
C21 C20 H20 118.9 .
C19 C20 H20 118.9 .
C22 C21 C20 119.2(3) .
C22 C21 H21 120.4 .
C20 C21 H21 120.4 .
C21 C22 C23 121.5(3) .
C21 C22 H22 119.2 .
C23 C22 H22 119.2 .
C22 C23 C18 118.6(3) .
C22 C23 C27 121.3(3) .
C18 C23 C27 120.0(3) .
C19 C24 C26 110.9(3) .
C19 C24 C25 112.1(2) .
C26 C24 C25 110.1(2) .
C19 C24 H24 107.9 .
C26 C24 H24 107.9 .
C25 C24 H24 107.9 .
C24 C25 H25C 109.5 .
C24 C25 H25B 109.5 .
H25C C25 H25B 109.5 .
C24 C25 H25A 109.5 .
H25C C25 H25A 109.5 .
H25B C25 H25A 109.5 .
C24 C26 H26C 109.5 .
C24 C26 H26B 109.5 .
H26C C26 H26B 109.5 .
C24 C26 H26A 109.5 .
H26C C26 H26A 109.5 .
H26B C26 H26A 109.5 .
C23 C27 C29 113.6(3) .
C23 C27 C28 110.6(3) .
C29 C27 C28 110.9(3) .
C23 C27 H27 107.1 .
C29 C27 H27 107.1 .
C28 C27 H27 107.1 .
C27 C28 H28C 109.5 .
C27 C28 H28B 109.5 .
H28C C28 H28B 109.5 .
C27 C28 H28A 109.5 .
H28C C28 H28A 109.5 .
H28B C28 H28A 109.5 .
C27 C29 H29C 109.5 .
C27 C29 H29B 109.5 .
H29C C29 H29B 109.5 .
C27 C29 H29A 109.5 .
H29C C29 H29A 109.5 .
H29B C29 H29A 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hg C2 2.128(3) .
Hg C2 2.128(3) 10_655
N1 C1 1.277(3) .
N1 C6 1.428(3) .
N2 C3 1.272(3) .
N2 C18 1.430(3) .
C1 C2 1.500(4) .
C1 C4 1.505(4) .
C2 C3 1.501(4) .
C2 H2 1 .
C3 C5 1.510(4) .
C4 H4C 0.98 .
C4 H4B 0.98 .
C4 H4A 0.98 .
C5 H5C 0.98 .
C5 H5B 0.98 .
C5 H5A 0.98 .
C6 C7 1.401(4) .
C6 C11 1.402(4) .
C7 C8 1.389(4) .
C7 C12 1.521(4) .
C8 C9 1.382(5) .
C8 H8 0.95 .
C9 C10 1.361(5) .
C9 H9 0.95 .
C10 C11 1.392(4) .
C10 H10 0.95 .
C11 C15 1.516(4) .
C12 C13 1.519(5) .
C12 C14 1.527(5) .
C12 H12 1 .
C13 H13C 0.98 .
C13 H13B 0.98 .
C13 H13A 0.98 .
C14 H14C 0.98 .
C14 H14B 0.98 .
C14 H14A 0.98 .
C15 C17 1.518(5) .
C15 C16 1.543(5) .
C15 H15 1 .
C16 H16C 0.98 .
C16 H16B 0.98 .
C16 H16A 0.98 .
C17 H17C 0.98 .
C17 H17B 0.98 .
C17 H17A 0.98 .
C18 C19 1.408(4) .
C18 C23 1.409(4) .
C19 C20 1.393(4) .
C19 C24 1.516(4) .
C20 C21 1.382(4) .
C20 H20 0.95 .
C21 C22 1.378(4) .
C21 H21 0.95 .
C22 C23 1.389(4) .
C22 H22 0.95 .
C23 C27 1.514(4) .
C24 C26 1.528(4) .
C24 C25 1.528(4) .
C24 H24 1 .
C25 H25C 0.98 .
C25 H25B 0.98 .
C25 H25A 0.98 .
C26 H26C 0.98 .
C26 H26B 0.98 .
C26 H26A 0.98 .
C27 C29 1.517(5) .
C27 C28 1.523(5) .
C27 H27 1 .
C28 H28C 0.98 .
C28 H28B 0.98 .
C28 H28A 0.98 .
C29 H29C 0.98 .
C29 H29B 0.98 .
C29 H29A 0.98 .
