#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:32:45 +0100 (vie 25 de mar de 2016) $
#$Revision: 179753 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/49/7004979.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_7004979
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Merle, Philippe G.'
_publ_section_title
;
 Synthesis and structures of selected benzamidinates of Li, Na, Al, Zr
 and Sn(II) using the C1-symmetric ligands [N(SiMe3)C(C6H4Me-4 or
 Ph)NPh]-.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              585
_journal_page_last               594
_journal_paper_doi               10.1039/b614351b
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H31 Li1 N2 O1 Si1'
_chemical_formula_structural     'C21 H31 LI1 N2 O1 SI1'
_chemical_formula_sum            'C42 H62 Li2 N4 O2 Si2'
_chemical_formula_weight         725.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             1999-04-12T13:28:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.97(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.861(7)
_cell_length_b                   9.412(4)
_cell_length_c                   23.889(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      8.5
_cell_measurement_theta_min      7.3
_cell_measurement_wavelength     0.71073
_cell_volume                     2209(2)
_computing_cell_refinement       'CAD4 (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'CAMERON (Watkin,Pearce & Prout, 1993)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.24976E-1
_diffrn_orient_matrix_UB_12      0.00667
_diffrn_orient_matrix_UB_13      0.41391E-1
_diffrn_orient_matrix_UB_21      0.6839E-2
_diffrn_orient_matrix_UB_22      0.105664
_diffrn_orient_matrix_UB_23      -0.3143E-2
_diffrn_orient_matrix_UB_31      -0.98447E-1
_diffrn_orient_matrix_UB_32      0.8839E-2
_diffrn_orient_matrix_UB_33      0.6515E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            4096
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        7
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.09
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.199
_refine_ls_wR_factor_ref         0.2272
_reflns_number_gt                2671
_reflns_number_total             3866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b614351b.txt
_cod_data_source_block           (1)-apr799
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7004979
#BEGIN Tags that were not found in dictionaries:
_diffrn_standards_decay_corr_max 1.073
_diffrn_standards_decay_corr_min 0.996
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Li Li 0.0853(6) 0.0208(5) -0.03721(19) 0.0364(12) Uani 1 1 d . . .
Si Si 0.03853(10) -0.23878(9) -0.14290(3) 0.0401(3) Uani 1 1 d . A .
O O 0.1835(3) 0.1711(2) -0.07294(10) 0.0528(7) Uani 1 1 d . . .
N1 N -0.1377(3) 0.0323(3) -0.04543(9) 0.0333(6) Uani 1 1 d . . .
N2 N -0.0049(3) -0.1113(3) -0.09621(10) 0.0354(6) Uani 1 1 d . . .
C1 C -0.1187(3) -0.0414(3) -0.09298(11) 0.0315(7) Uani 1 1 d . A .
C2 C -0.2325(3) -0.0451(3) -0.13941(11) 0.0333(7) Uani 1 1 d . . .
C3 C -0.3515(4) -0.1166(4) -0.13366(14) 0.0520(10) Uani 1 1 d . A .
H3 H -0.3647 -0.1606 -0.0988 0.062 Uiso 1 1 calc R . .
C4 C -0.4529(4) -0.1264(5) -0.17716(15) 0.0571(10) Uani 1 1 d . . .
H4 H -0.5335 -0.1782 -0.1719 0.068 Uiso 1 1 calc R A .
C5 C -0.4387(4) -0.0617(4) -0.22850(14) 0.0488(9) Uani 1 1 d . A .
C6 C -0.3210(4) 0.0120(4) -0.23369(14) 0.0529(10) Uani 1 1 d . . .
H6 H -0.3095 0.059 -0.2681 0.064 Uiso 1 1 calc R A .
C7 C -0.2179(4) 0.0207(4) -0.19059(13) 0.0456(9) Uani 1 1 d . A .
H7 H -0.137 0.0718 -0.1961 0.055 Uiso 1 1 calc R . .
C8 C -0.5488(4) -0.0719(6) -0.27654(17) 0.0741(14) Uani 1 1 d . . .
H8A H -0.6329 -0.0294 -0.2652 0.111 Uiso 0.5 1 calc PR A .
H8B H -0.565 -0.172 -0.2863 0.111 Uiso 0.5 1 calc PR . .
H8C H -0.5197 -0.0211 -0.3092 0.111 Uiso 0.5 1 calc PR . .
H8D H -0.5122 -0.1189 -0.3086 0.111 Uiso 0.5 1 calc PR . .
H8E H -0.58 0.0237 -0.2875 0.111 Uiso 0.5 1 calc PR . .
H8F H -0.6254 -0.1272 -0.2646 0.111 Uiso 0.5 1 calc PR . .
C9 C -0.2410(3) 0.1368(3) -0.04675(12) 0.0344(7) Uani 1 1 d . A .
C10 C -0.3471(4) 0.1255(4) -0.01277(14) 0.0513(9) Uani 1 1 d . . .
H10 H -0.3548 0.043 0.0096 0.062 Uiso 1 1 calc R A .
C11 C -0.4429(4) 0.2341(5) -0.01108(17) 0.0671(12) Uani 1 1 d . A .
H11 H -0.515 0.225 0.0126 0.081 Uiso 1 1 calc R . .
C12 C -0.4339(4) 0.3544(4) -0.04331(17) 0.0590(11) Uani 1 1 d . . .
H12 H -0.4993 0.4282 -0.042 0.071 Uiso 1 1 calc R A .
C13 C -0.3302(4) 0.3665(4) -0.07714(16) 0.0509(9) Uani 1 1 d . A .
H13 H -0.3232 0.4491 -0.0995 0.061 Uiso 1 1 calc R . .
C14 C -0.2352(4) 0.2594(3) -0.07911(14) 0.0419(8) Uani 1 1 d . . .
H14 H -0.164 0.2695 -0.1032 0.05 Uiso 1 1 calc R A .
C15 C -0.0890(4) -0.3850(4) -0.15385(17) 0.0647(12) Uani 1 1 d . . .
H15A H -0.0522 -0.4604 -0.1764 0.097 Uiso 1 1 calc R A .
H15B H -0.1729 -0.3477 -0.1735 0.097 Uiso 1 1 calc R . .
H15C H -0.1089 -0.4236 -0.1174 0.097 Uiso 1 1 calc R . .
C16 C 0.0737(5) -0.1687(4) -0.21367(14) 0.0621(11) Uani 1 1 d . . .
H16A H -0.011 -0.1328 -0.2332 0.093 Uiso 1 1 calc R A .
H16B H 0.1101 -0.2452 -0.2358 0.093 Uiso 1 1 calc R . .
H16C H 0.1403 -0.0915 -0.209 0.093 Uiso 1 1 calc R . .
C17 C 0.2012(4) -0.3174(4) -0.11147(16) 0.0542(10) Uani 1 1 d . . .
H17A H 0.2343 -0.3872 -0.1375 0.081 Uiso 1 1 calc R A .
H17B H 0.1856 -0.3643 -0.076 0.081 Uiso 1 1 calc R . .
H17C H 0.2691 -0.2421 -0.1044 0.081 Uiso 1 1 calc R . .
C18 C 0.1767(5) 0.3182(4) -0.06071(19) 0.0630(11) Uani 1 1 d . A .
H18A H 0.1128 0.3656 -0.0891 0.076 Uiso 1 1 calc R . .
H18B H 0.2677 0.3618 -0.0623 0.076 Uiso 1 1 calc R . .
C19 C 0.1306(5) 0.3379(4) -0.00505(18) 0.0747(14) Uani 1 1 d . . .
H19A H 0.1967 0.2953 0.0231 0.112 Uiso 1 1 calc R A .
H19B H 0.0419 0.2919 -0.0033 0.112 Uiso 1 1 calc R . .
H19C H 0.1222 0.4396 0.0026 0.112 Uiso 1 1 calc R . .
C20 C 0.2697(7) 0.1367(6) -0.1189(3) 0.052(2) Uani 0.745(16) 1 d P A 1
H20A H 0.2768 0.0323 -0.1226 0.063 Uiso 0.745(16) 1 calc PR A 1
H20B H 0.3624 0.175 -0.1097 0.063 Uiso 0.745(16) 1 calc PR A 1
C21 C 0.2114(12) 0.1982(8) -0.1734(3) 0.085(3) Uani 0.745(16) 1 d P A 1
H21A H 0.2705 0.1746 -0.203 0.128 Uiso 0.745(16) 1 calc PR A 1
H21B H 0.205 0.3017 -0.1699 0.128 Uiso 0.745(16) 1 calc PR A 1
H21C H 0.1205 0.1586 -0.1831 0.128 Uiso 0.745(16) 1 calc PR A 1
C20A C 0.162(4) 0.184(3) -0.1350(9) 0.110(11) Uani 0.255(16) 1 d P A 2
H20C H 0.1122 0.2725 -0.1463 0.132 Uiso 0.255(16) 1 calc PR A 2
H20D H 0.1121 0.1015 -0.152 0.132 Uiso 0.255(16) 1 calc PR A 2
C21A C 0.305(3) 0.189(4) -0.1507(12) 0.102(10) Uani 0.255(16) 1 d P A 2
H21D H 0.3049 0.2065 -0.1912 0.153 Uiso 0.255(16) 1 calc PR A 2
H21E H 0.3495 0.0977 -0.1415 0.153 Uiso 0.255(16) 1 calc PR A 2
H21F H 0.3545 0.2651 -0.1299 0.153 Uiso 0.255(16) 1 calc PR A 2
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'
Li Li -0.0003 0.0001 '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'
O O 0.0106 0.006 '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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 -2 6
-2 3 5
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
O Li N2 110.2(2) . . ?
O Li N1 120.2(3) . 3 ?
N2 Li N1 125.3(3) . 3 ?
O Li N1 117.2(3) . . ?
N2 Li N1 65.92(19) . . ?
N1 Li N1 105.3(2) 3 . ?
O Li C1 111.1(2) . . ?
N2 Li C1 33.24(13) . . ?
N1 Li C1 127.2(3) 3 . ?
N1 Li C1 34.15(12) . . ?
O Li Li 142.0(4) . 3 ?
N2 Li Li 96.5(3) . 3 ?
N1 Li Li 55.04(19) 3 3 ?
N1 Li Li 50.3(2) . 3 ?
C1 Li Li 77.3(3) . 3 ?
N2 Si C17 105.66(15) . . ?
N2 Si C15 113.77(16) . . ?
C17 Si C15 108.0(2) . . ?
N2 Si C16 114.56(15) . . ?
C17 Si C16 106.45(19) . . ?
C15 Si C16 107.9(2) . . ?
C18 O C20 114.0(3) . . ?
C18 O C20A 96.8(12) . . ?
C20 O C20A 47.1(13) . . ?
C18 O Li 125.7(3) . . ?
C20 O Li 120.3(3) . . ?
C20A O Li 117.7(11) . . ?
C1 N1 C9 119.2(2) . . ?
C1 N1 Li 129.6(2) . 3 ?
C9 N1 Li 108.1(2) . 3 ?
C1 N1 Li 80.8(2) . . ?
C9 N1 Li 138.6(2) . . ?
Li N1 Li 74.7(2) 3 . ?
C1 N2 Si 130.7(2) . . ?
C1 N2 Li 88.7(2) . . ?
Si N2 Li 139.6(2) . . ?
N2 C1 N1 119.1(3) . . ?
N2 C1 C2 122.1(2) . . ?
N1 C1 C2 118.7(3) . . ?
N2 C1 Li 58.0(2) . . ?
N1 C1 Li 65.1(2) . . ?
C2 C1 Li 162.4(2) . . ?
C3 C2 C7 117.5(3) . . ?
C3 C2 C1 121.8(3) . . ?
C7 C2 C1 120.7(3) . . ?
C2 C3 C4 121.9(3) . . ?
C3 C4 C5 120.9(3) . . ?
C6 C5 C4 117.0(3) . . ?
C6 C5 C8 121.5(3) . . ?
C4 C5 C8 121.5(4) . . ?
C5 C6 C7 122.5(3) . . ?
C6 C7 C2 120.2(3) . . ?
C10 C9 C14 117.3(3) . . ?
C10 C9 N1 120.9(3) . . ?
C14 C9 N1 121.6(3) . . ?
C9 C10 C11 120.6(4) . . ?
C12 C11 C10 120.7(4) . . ?
C13 C12 C11 119.2(4) . . ?
C12 C13 C14 120.4(4) . . ?
C13 C14 C9 121.7(3) . . ?
O C18 C19 109.7(3) . . ?
O C20 C21 111.1(7) . . ?
O C20A C21A 101(3) . . ?
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
Li O 1.953(5) . ?
Li N2 2.026(6) . ?
Li N1 2.058(5) 3 ?
Li N1 2.193(6) . ?
Li C1 2.387(6) . ?
Li Li 2.581(10) 3 ?
Si N2 1.718(3) . ?
Si C17 1.864(4) . ?
Si C15 1.867(4) . ?
Si C16 1.875(4) . ?
O C18 1.418(4) . ?
O C20 1.482(6) . ?
O C20A 1.48(2) . ?
N1 C1 1.357(4) . ?
N1 C9 1.415(4) . ?
N1 Li 2.058(5) 3 ?
N2 C1 1.309(4) . ?
C1 C2 1.508(4) . ?
C2 C3 1.370(5) . ?
C2 C7 1.389(4) . ?
C3 C4 1.381(5) . ?
C4 C5 1.387(5) . ?
C5 C6 1.367(5) . ?
C5 C8 1.513(5) . ?
C6 C7 1.385(5) . ?
C9 C10 1.383(5) . ?
C9 C14 1.392(4) . ?
C10 C11 1.395(6) . ?
C11 C12 1.377(6) . ?
C12 C13 1.362(5) . ?
C13 C14 1.379(5) . ?
C18 C19 1.454(6) . ?
C20 C21 1.492(12) . ?
C20A C21A 1.49(5) . ?
