#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:06:22 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180060 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/06/7050600.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_7050600
loop_
_publ_author_name
'Kay Lee, Hung'
'Suet Lam, Tung'
'Lam, Chi-Keung'
'Li, Hung-Wing'
'Man Fung, Sze'
_publ_section_title
;
 Synthesis and structural characterisation of divalent transition metal
 complexes containing an unsymmetrical benzamidinate ligandElectronic
 supplementary information (ESI) available: inclination angles in
 complexes 1?6. See http://www.rsc.org/suppdata/nj/b3/b303527a//
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1310
_journal_paper_doi               10.1039/b303527a
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C36 H46 N4 Ni Si2'
_chemical_formula_weight         649.66
_chemical_name_systematic
;
?
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.9800(10)
_cell_angle_beta                 109.071(2)
_cell_angle_gamma                114.9160(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3641(9)
_cell_length_b                   12.4981(9)
_cell_length_c                   14.4849(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1816.0(2)
_computing_cell_refinement       'Bruker SMART CCD Diffractometer'
_computing_data_collection       'Bruker SMART CCD Diffractometer'
_computing_data_reduction        'Bruker SMART CCD Diffractometer'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHLEXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART CCD Diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0134
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12250
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7930
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0077(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         8591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0688P)²+0.1234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                6473
_reflns_number_total             8591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303527a.txt
_cod_data_source_block           Compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050600
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.76947(2) 0.69282(2) 0.702904(19) 0.03747(10) Uani 1 1 d . . .
Si1 Si 0.87505(6) 0.48196(6) 0.74811(6) 0.05528(18) Uani 1 1 d . . .
N1 N 0.61129(15) 0.58302(15) 0.71051(14) 0.0431(4) Uani 1 1 d . . .
C1 C 0.66449(19) 0.51664(18) 0.74581(16) 0.0425(4) Uani 1 1 d . . .
Si2 Si 0.65399(6) 0.89283(6) 0.63323(5) 0.04880(16) Uani 1 1 d . . .
N2 N 0.77761(16) 0.55084(15) 0.73788(15) 0.0469(4) Uani 1 1 d . . .
C2 C 0.6071(2) 0.4206(2) 0.79260(19) 0.0511(5) Uani 1 1 d . . .
N3 N 0.93564(15) 0.81332(15) 0.71089(14) 0.0447(4) Uani 1 1 d . . .
C3 C 0.4953(3) 0.3096(3) 0.7353(2) 0.0802(9) Uani 1 1 d . . .
H3A H 0.4516 0.2924 0.6647 0.096 Uiso 1 1 calc R . .
N4 N 0.76378(16) 0.83874(15) 0.67702(14) 0.0446(4) Uani 1 1 d . . .
C4 C 0.4452(3) 0.2206(3) 0.7810(3) 0.0968(11) Uani 1 1 d . . .
H4A H 0.3683 0.1449 0.7409 0.116 Uiso 1 1 calc R . .
C5 C 0.5075(4) 0.2442(4) 0.8820(3) 0.1279(16) Uani 1 1 d . . .
H5A H 0.4722 0.1865 0.9131 0.154 Uiso 1 1 calc R . .
C6 C 0.6241(5) 0.3540(4) 0.9402(3) 0.167(3) Uani 1 1 d . . .
H6A H 0.6693 0.3698 1.0103 0.201 Uiso 1 1 calc R . .
C7 C 0.6740(4) 0.4410(3) 0.8941(3) 0.1195(16) Uani 1 1 d . . .
H7A H 0.7542 0.5142 0.9332 0.143 Uiso 1 1 calc R . .
C8 C 0.50681(19) 0.58939(18) 0.72787(16) 0.0413(4) Uani 1 1 d . . .
C9 C 0.5359(2) 0.6732(2) 0.81841(19) 0.0537(5) Uani 1 1 d . . .
C10 C 0.4328(3) 0.6838(3) 0.8299(2) 0.0712(7) Uani 1 1 d . . .
H10A H 0.4503 0.7398 0.8895 0.085 Uiso 1 1 calc R . .
C11 C 0.3057(3) 0.6126(3) 0.7544(2) 0.0717(8) Uani 1 1 d . . .
H11A H 0.2380 0.6206 0.7633 0.086 Uiso 1 1 calc R . .
C12 C 0.2785(2) 0.5308(2) 0.6666(2) 0.0615(6) Uani 1 1 d . . .
H12A H 0.1918 0.4826 0.6165 0.074 Uiso 1 1 calc R . .
C13 C 0.3780(2) 0.51741(19) 0.65025(18) 0.0468(5) Uani 1 1 d . . .
C14 C 0.3456(2) 0.4315(2) 0.5503(2) 0.0642(7) Uani 1 1 d . . .
H14A H 0.2525 0.3907 0.5075 0.096 Uiso 1 1 calc R . .
H14B H 0.3707 0.3702 0.5635 0.096 Uiso 1 1 calc R . .
H14C H 0.3930 0.4785 0.5158 0.096 Uiso 1 1 calc R . .
C15 C 0.6744(3) 0.7517(3) 0.9013(2) 0.0837(9) Uani 1 1 d . . .
H15A H 0.7325 0.7325 0.8811 0.126 Uiso 1 1 calc R . .
H15B H 0.6778 0.7345 0.9645 0.126 Uiso 1 1 calc R . .
H15C H 0.7016 0.8382 0.9115 0.126 Uiso 1 1 calc R . .
C16 C 0.9189(3) 0.4870(3) 0.6376(3) 0.0871(9) Uani 1 1 d . . .
H16A H 0.9636 0.5718 0.6393 0.131 Uiso 1 1 calc R . .
H16B H 0.8400 0.4394 0.5743 0.131 Uiso 1 1 calc R . .
H16C H 0.9757 0.4523 0.6420 0.131 Uiso 1 1 calc R . .
C17 C 0.7889(3) 0.3164(2) 0.7424(3) 0.0939(11) Uani 1 1 d . . .
H17A H 0.7090 0.2700 0.6797 0.141 Uiso 1 1 calc R . .
H17B H 0.7679 0.3121 0.8005 0.141 Uiso 1 1 calc R . .
H17C H 0.8453 0.2817 0.7441 0.141 Uiso 1 1 calc R . .
C18 C 1.0284(3) 0.5681(3) 0.8699(3) 0.0857(9) Uani 1 1 d . . .
H18A H 1.0745 0.6539 0.8743 0.129 Uiso 1 1 calc R . .
H18B H 1.0836 0.5321 0.8710 0.129 Uiso 1 1 calc R . .
H18C H 1.0064 0.5629 0.9275 0.129 Uiso 1 1 calc R . .
C21 C 0.89289(19) 0.89380(19) 0.70374(17) 0.0445(5) Uani 1 1 d . . .
C22 C 0.9813(2) 1.0310(2) 0.7294(2) 0.0563(6) Uani 1 1 d . . .
C23 C 1.0494(3) 1.0760(3) 0.6722(3) 0.0965(11) Uani 1 1 d . . .
H23A H 1.0416 1.0215 0.6165 0.116 Uiso 1 1 calc R . .
C24 C 1.1305(4) 1.2049(4) 0.6991(5) 0.1332(19) Uani 1 1 d . . .
H24A H 1.1759 1.2362 0.6603 0.160 Uiso 1 1 calc R . .
C25 C 1.1434(4) 1.2848(4) 0.7813(5) 0.133(2) Uani 1 1 d . . .
H25A H 1.1981 1.3701 0.7987 0.159 Uiso 1 1 calc R . .
C26 C 1.0760(4) 1.2401(3) 0.8387(3) 0.1110(14) Uani 1 1 d . . .
H26A H 1.0852 1.2947 0.8951 0.133 Uiso 1 1 calc R . .
C27 C 0.9942(3) 1.1126(2) 0.8118(2) 0.0768(8) Uani 1 1 d . . .
H27A H 0.9476 1.0820 0.8499 0.092 Uiso 1 1 calc R . .
C28 C 1.07215(19) 0.84962(18) 0.76112(19) 0.0479(5) Uani 1 1 d . . .
C29 C 1.1357(2) 0.8878(2) 0.8680(2) 0.0600(6) Uani 1 1 d . . .
C30 C 1.2689(3) 0.9209(3) 0.9143(3) 0.0847(10) Uani 1 1 d . . .
H30A H 1.3132 0.9468 0.9859 0.102 Uiso 1 1 calc R . .
C31 C 1.3345(3) 0.9155(3) 0.8559(4) 0.0984(13) Uani 1 1 d . . .
H31A H 1.4233 0.9389 0.8878 0.118 Uiso 1 1 calc R . .
C32 C 1.2712(3) 0.8764(3) 0.7514(3) 0.0849(10) Uani 1 1 d . . .
H32A H 1.3174 0.8724 0.7129 0.102 Uiso 1 1 calc R . .
C33 C 1.1383(2) 0.8418(2) 0.7000(2) 0.0627(7) Uani 1 1 d . . .
C34 C 1.0707(3) 0.7969(3) 0.5846(3) 0.0908(10) Uani 1 1 d . . .
H34A H 1.1324 0.7983 0.5575 0.136 Uiso 1 1 calc R . .
H34B H 1.0380 0.8502 0.5614 0.136 Uiso 1 1 calc R . .
H34C H 0.9984 0.7132 0.5608 0.136 Uiso 1 1 calc R . .
C35 C 1.0637(3) 0.8908(3) 0.9328(2) 0.0781(8) Uani 1 1 d . . .
H35A H 0.9740 0.8658 0.8890 0.117 Uiso 1 1 calc R . .
H35B H 1.1062 0.9739 0.9792 0.117 Uiso 1 1 calc R . .
H35C H 1.0646 0.8348 0.9718 0.117 Uiso 1 1 calc R . .
C36 C 0.6375(3) 0.9761(3) 0.7400(3) 0.0807(8) Uani 1 1 d . . .
H36A H 0.6116 0.9225 0.7794 0.121 Uiso 1 1 calc R . .
H36B H 0.5717 0.9990 0.7118 0.121 Uiso 1 1 calc R . .
H36C H 0.7206 1.0497 0.7839 0.121 Uiso 1 1 calc R . .
C37 C 0.7043(3) 0.9950(3) 0.5556(2) 0.0765(8) Uani 1 1 d . . .
H37A H 0.7123 0.9510 0.5007 0.115 Uiso 1 1 calc R . .
H37B H 0.7876 1.0687 0.5991 0.115 Uiso 1 1 calc R . .
H37C H 0.6388 1.0181 0.5270 0.115 Uiso 1 1 calc R . .
C38 C 0.4884(2) 0.7562(3) 0.5475(2) 0.0740(8) Uani 1 1 d . . .
H38A H 0.4601 0.7019 0.5858 0.111 Uiso 1 1 calc R . .
H38B H 0.4932 0.7120 0.4906 0.111 Uiso 1 1 calc R . .
H38C H 0.4265 0.7842 0.5219 0.111 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 0.0000 0.0000 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 173.70(8) . . ?
N1 Ni1 N4 110.27(7) . . ?
N3 Ni1 N4 69.09(7) . . ?
N1 Ni1 N2 68.93(7) . . ?
N3 Ni1 N2 111.28(7) . . ?
N4 Ni1 N2 176.39(8) . . ?
N1 Ni1 C21 143.52(7) . . ?
N3 Ni1 C21 34.66(7) . . ?
N4 Ni1 C21 34.94(7) . . ?
N2 Ni1 C21 144.83(7) . . ?
N1 Ni1 C1 34.52(7) . . ?
N3 Ni1 C1 144.57(7) . . ?
N4 Ni1 C1 143.87(7) . . ?
N2 Ni1 C1 34.81(7) . . ?
C21 Ni1 C1 165.57(7) . . ?
N2 Si1 C16 106.99(12) . . ?
N2 Si1 C18 111.20(13) . . ?
C16 Si1 C18 109.10(16) . . ?
N2 Si1 C17 113.11(11) . . ?
C16 Si1 C17 108.21(16) . . ?
C18 Si1 C17 108.13(15) . . ?
C1 N1 C8 124.89(17) . . ?
C1 N1 Ni1 90.42(12) . . ?
C8 N1 Ni1 137.87(13) . . ?
N1 C1 N2 110.86(18) . . ?
N1 C1 C2 123.85(18) . . ?
N2 C1 C2 125.23(19) . . ?
N1 C1 Ni1 55.07(10) . . ?
N2 C1 Ni1 56.64(10) . . ?
C2 C1 Ni1 169.32(16) . . ?
N4 Si2 C36 112.58(13) . . ?
N4 Si2 C38 108.17(11) . . ?
C36 Si2 C38 107.37(14) . . ?
N4 Si2 C37 110.47(11) . . ?
C36 Si2 C37 110.29(14) . . ?
C38 Si2 C37 107.76(14) . . ?
C1 N2 Si1 132.10(15) . . ?
C1 N2 Ni1 88.55(12) . . ?
Si1 N2 Ni1 139.22(10) . . ?
C7 C2 C3 118.8(2) . . ?
C7 C2 C1 118.9(2) . . ?
C3 C2 C1 122.1(2) . . ?
C21 N3 C28 123.35(17) . . ?
C21 N3 Ni1 89.47(12) . . ?
C28 N3 Ni1 138.57(14) . . ?
C2 C3 C4 120.8(3) . . ?
C21 N4 Si2 129.78(15) . . ?
C21 N4 Ni1 88.53(12) . . ?
Si2 N4 Ni1 141.63(10) . . ?
C5 C4 C3 120.0(3) . . ?
C4 C5 C6 119.7(3) . . ?
C5 C6 C7 119.9(4) . . ?
C2 C7 C6 120.5(3) . . ?
C9 C8 C13 121.25(19) . . ?
C9 C8 N1 119.55(19) . . ?
C13 C8 N1 119.05(19) . . ?
C8 C9 C10 118.2(2) . . ?
C8 C9 C15 121.4(2) . . ?
C10 C9 C15 120.4(2) . . ?
C11 C10 C9 120.9(2) . . ?
C12 C11 C10 120.3(2) . . ?
C11 C12 C13 121.3(2) . . ?
C8 C13 C12 118.0(2) . . ?
C8 C13 C14 122.09(19) . . ?
C12 C13 C14 119.9(2) . . ?
N3 C21 N4 111.32(17) . . ?
N3 C21 C22 123.74(18) . . ?
N4 C21 C22 124.83(19) . . ?
N3 C21 Ni1 55.87(10) . . ?
N4 C21 Ni1 56.54(10) . . ?
C22 C21 Ni1 167.37(17) . . ?
C27 C22 C23 119.8(3) . . ?
C27 C22 C21 119.0(2) . . ?
C23 C22 C21 121.3(3) . . ?
C22 C23 C24 119.1(4) . . ?
C25 C24 C23 120.6(4) . . ?
C24 C25 C26 120.4(3) . . ?
C25 C26 C27 119.3(4) . . ?
C22 C27 C26 120.8(3) . . ?
C29 C28 C33 121.3(2) . . ?
C29 C28 N3 120.0(2) . . ?
C33 C28 N3 118.6(2) . . ?
C28 C29 C30 118.4(3) . . ?
C28 C29 C35 121.2(2) . . ?
C30 C29 C35 120.3(3) . . ?
C31 C30 C29 120.8(3) . . ?
C32 C31 C30 120.4(3) . . ?
C31 C32 C33 121.8(3) . . ?
C32 C33 C28 117.2(3) . . ?
C32 C33 C34 120.5(3) . . ?
C28 C33 C34 122.3(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.9083(15) . ?
Ni1 N3 1.9214(16) . ?
Ni1 N4 1.9370(17) . ?
Ni1 N2 1.9448(17) . ?
Ni1 C21 2.321(2) . ?
Ni1 C1 2.328(2) . ?
Si1 N2 1.7341(17) . ?
Si1 C16 1.850(3) . ?
Si1 C18 1.853(3) . ?
Si1 C17 1.860(3) . ?
N1 C1 1.319(3) . ?
N1 C8 1.426(2) . ?
C1 N2 1.329(2) . ?
C1 C2 1.492(3) . ?
Si2 N4 1.7412(18) . ?
Si2 C36 1.858(3) . ?
Si2 C38 1.858(3) . ?
Si2 C37 1.862(3) . ?
C2 C7 1.354(4) . ?
C2 C3 1.356(3) . ?
N3 C21 1.320(3) . ?
N3 C28 1.430(3) . ?
C3 C4 1.397(4) . ?
N4 C21 1.330(2) . ?
C4 C5 1.332(5) . ?
C5 C6 1.375(5) . ?
C6 C7 1.383(5) . ?
C8 C9 1.392(3) . ?
C8 C13 1.397(3) . ?
C9 C10 1.396(3) . ?
C9 C15 1.500(4) . ?
C10 C11 1.373(4) . ?
C11 C12 1.358(4) . ?
C12 C13 1.397(3) . ?
C13 C14 1.495(3) . ?
C21 C22 1.500(3) . ?
C22 C27 1.376(4) . ?
C22 C23 1.377(4) . ?
C23 C24 1.401(5) . ?
C24 C25 1.360(7) . ?
C25 C26 1.374(7) . ?
C26 C27 1.388(4) . ?
C28 C29 1.387(4) . ?
C28 C33 1.406(3) . ?
C29 C30 1.401(4) . ?
C29 C35 1.498(4) . ?
C30 C31 1.363(5) . ?
C31 C32 1.356(5) . ?
C32 C33 1.398(4) . ?
C33 C34 1.496(4) . ?
