#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:51:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179266 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/86/4318678.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_4318678
loop_
_publ_author_name
'Wilda Vargas'
'Ulrich Englich'
'Karin Ruhlandt-Senge'
_publ_section_title
;
 A Novel Group of Alkaline Earth Metal Amides: Syntheses and
 Characterization of M[N(2,6-iPr2C6H3)(SiMe3)]2(THF)2 (M = Mg, Ca, Sr, Ba)
 and the Linear, Two-Coordinate Mg[N(2,6-iPr2C6H3)(SiMe3)]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5602
_journal_page_last               5608
_journal_paper_doi               10.1021/ic0203668
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C30 H52 Mg N2 Si2'
_chemical_formula_weight         521.23
_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                96.4870(10)
_cell_angle_beta                 94.5370(10)
_cell_angle_gamma                98.2220(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4687(6)
_cell_length_b                   9.6818(6)
_cell_length_c                   17.9296(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1608.77(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10438
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'R. Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         7197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0456
_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)+(0.0706P)²+1.1636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                6636
_reflns_number_total             7197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203668_1.cif
_cod_data_source_block           wilda
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318678
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
Si1 Si 0.74761(4) 0.73601(4) 0.49095(2) 0.01937(11) Uani 1 1 d . . .
Mg1 Mg 0.5000 0.5000 0.5000 0.02503(18) Uani 1 2 d S . .
N1 N 0.61782(13) 0.61229(13) 0.43986(7) 0.0168(2) Uani 1 1 d . . .
C1 C 0.60247(15) 0.58801(15) 0.35940(8) 0.0159(3) Uani 1 1 d . . .
C2 C 0.51025(16) 0.66076(16) 0.31726(9) 0.0187(3) Uani 1 1 d . . .
C6 C 0.67449(16) 0.48758(15) 0.32065(8) 0.0180(3) Uani 1 1 d . . .
C5 C 0.65477(18) 0.46312(18) 0.24212(9) 0.0244(3) Uani 1 1 d . . .
H5A H 0.7026 0.3975 0.2168 0.029 Uiso 1 1 calc R . .
C7 C 0.42676(17) 0.76587(17) 0.35673(9) 0.0234(3) Uani 1 1 d . . .
H7A H 0.4817 0.8046 0.4050 0.028 Uiso 1 1 calc R . .
C3 C 0.49323(18) 0.63209(18) 0.23862(9) 0.0250(3) Uani 1 1 d . . .
H3A H 0.4325 0.6792 0.2110 0.030 Uiso 1 1 calc R . .
C8 C 0.76839(17) 0.40105(16) 0.36341(9) 0.0212(3) Uani 1 1 d . . .
H8A H 0.7948 0.4510 0.4144 0.025 Uiso 1 1 calc R . .
C4 C 0.56524(19) 0.53459(19) 0.20100(9) 0.0281(4) Uani 1 1 d . . .
H4A H 0.5536 0.5173 0.1486 0.034 Uiso 1 1 calc R . .
C12 C 0.90739(18) 0.3837(2) 0.32781(11) 0.0294(4) Uani 1 1 d . . .
H12A H 0.9590 0.4747 0.3232 0.044 Uiso 1 1 calc R . .
H12B H 0.8851 0.3304 0.2787 0.044 Uiso 1 1 calc R . .
H12C H 0.9653 0.3351 0.3591 0.044 Uiso 1 1 calc R . .
C15 C 0.93573(18) 0.7155(2) 0.47188(10) 0.0285(4) Uani 1 1 d . . .
H15A H 0.9914 0.8066 0.4721 0.043 Uiso 1 1 calc R . .
H15B H 0.9348 0.6614 0.4235 0.043 Uiso 1 1 calc R . .
H15C H 0.9774 0.6679 0.5103 0.043 Uiso 1 1 calc R . .
C10 C 0.4069(2) 0.8895(2) 0.31282(12) 0.0366(4) Uani 1 1 d . . .
H10A H 0.4988 0.9345 0.3020 0.055 Uiso 1 1 calc R . .
H10B H 0.3613 0.9559 0.3425 0.055 Uiso 1 1 calc R . .
H10C H 0.3482 0.8556 0.2664 0.055 Uiso 1 1 calc R . .
C11 C 0.6851(2) 0.2567(2) 0.37116(14) 0.0406(5) Uani 1 1 d . . .
H11A H 0.5981 0.2685 0.3936 0.061 Uiso 1 1 calc R . .
H11B H 0.7425 0.2079 0.4026 0.061 Uiso 1 1 calc R . .
H11C H 0.6623 0.2030 0.3222 0.061 Uiso 1 1 calc R . .
C13 C 0.7312(2) 0.9231(2) 0.48007(14) 0.0412(5) Uani 1 1 d . . .
H13A H 0.8248 0.9756 0.4787 0.062 Uiso 1 1 calc R . .
H13B H 0.6869 0.9633 0.5219 0.062 Uiso 1 1 calc R . .
H13C H 0.6735 0.9265 0.4340 0.062 Uiso 1 1 calc R . .
C14 C 0.7247(2) 0.7110(3) 0.59179(10) 0.0388(5) Uani 1 1 d . . .
H14A H 0.7950 0.7768 0.6243 0.058 Uiso 1 1 calc R . .
H14B H 0.7372 0.6169 0.5996 0.058 Uiso 1 1 calc R . .
H14C H 0.6304 0.7266 0.6030 0.058 Uiso 1 1 calc R . .
C9 C 0.2805(2) 0.6935(2) 0.37414(13) 0.0387(4) Uani 1 1 d . . .
H9A H 0.2935 0.6161 0.4018 0.058 Uiso 1 1 calc R . .
H9B H 0.2218 0.6592 0.3278 0.058 Uiso 1 1 calc R . .
H9C H 0.2346 0.7597 0.4038 0.058 Uiso 1 1 calc R . .
Si2 Si 0.25618(5) 1.12905(4) 0.11359(2) 0.01974(11) Uani 1 1 d . . .
Mg2 Mg 0.0000 1.0000 0.0000 0.0302(2) Uani 1 2 d S . .
N2 N 0.12401(14) 0.98782(13) 0.08788(7) 0.0181(3) Uani 1 1 d . . .
C16 C 0.10662(15) 0.85773(15) 0.11896(8) 0.0164(3) Uani 1 1 d . . .
C17 C 0.01874(16) 0.83780(16) 0.17849(8) 0.0187(3) Uani 1 1 d . . .
C20 C 0.14334(18) 0.61390(17) 0.11381(9) 0.0239(3) Uani 1 1 d . . .
H20A H 0.1854 0.5392 0.0930 0.029 Uiso 1 1 calc R . .
C21 C 0.17026(16) 0.74376(16) 0.08675(8) 0.0186(3) Uani 1 1 d . . .
C22 C -0.05207(17) 0.95608(17) 0.21506(9) 0.0224(3) Uani 1 1 d . . .
H22A H -0.0012 1.0445 0.2023 0.027 Uiso 1 1 calc R . .
C18 C -0.00665(18) 0.70480(17) 0.20294(9) 0.0233(3) Uani 1 1 d . . .
H18A H -0.0660 0.6908 0.2412 0.028 Uiso 1 1 calc R . .
C29 C 0.23883(19) 1.23906(19) 0.03388(11) 0.0294(4) Uani 1 1 d . . .
H29A H 0.3138 1.3187 0.0417 0.044 Uiso 1 1 calc R . .
H29B H 0.1474 1.2710 0.0324 0.044 Uiso 1 1 calc R . .
H29C H 0.2465 1.1834 -0.0130 0.044 Uiso 1 1 calc R . .
C23 C 0.26108(16) 0.75935(17) 0.02084(9) 0.0207(3) Uani 1 1 d . . .
H23A H 0.2944 0.8600 0.0211 0.025 Uiso 1 1 calc R . .
C19 C 0.05518(19) 0.59386(17) 0.17110(10) 0.0263(3) Uani 1 1 d . . .
H19A H 0.0377 0.5063 0.1880 0.032 Uiso 1 1 calc R . .
C30 C 0.44197(19) 1.0828(2) 0.12281(11) 0.0310(4) Uani 1 1 d . . .
H30A H 0.4980 1.1427 0.1642 0.047 Uiso 1 1 calc R . .
H30B H 0.4858 1.0956 0.0771 0.047 Uiso 1 1 calc R . .
H30C H 0.4372 0.9864 0.1318 0.047 Uiso 1 1 calc R . .
C28 C 0.2359(3) 1.2385(2) 0.20332(12) 0.0477(6) Uani 1 1 d . . .
H28A H 0.3283 1.2687 0.2309 0.072 Uiso 1 1 calc R . .
H28B H 0.1751 1.1839 0.2331 0.072 Uiso 1 1 calc R . .
H28C H 0.1938 1.3192 0.1922 0.072 Uiso 1 1 calc R . .
C27 C 0.3938(2) 0.6867(2) 0.02683(13) 0.0384(5) Uani 1 1 d . . .
H27A H 0.4490 0.7202 0.0743 0.058 Uiso 1 1 calc R . .
H27B H 0.4511 0.7074 -0.0135 0.058 Uiso 1 1 calc R . .
H27C H 0.3648 0.5869 0.0235 0.058 Uiso 1 1 calc R . .
C26 C 0.1725(2) 0.7067(3) -0.05456(10) 0.0402(5) Uani 1 1 d . . .
H26A H 0.0893 0.7528 -0.0580 0.060 Uiso 1 1 calc R . .
H26B H 0.1429 0.6069 -0.0580 0.060 Uiso 1 1 calc R . .
H26C H 0.2294 0.7272 -0.0951 0.060 Uiso 1 1 calc R . .
C24 C -0.2081(2) 0.9449(3) 0.18382(17) 0.0611(8) Uani 1 1 d . . .
H24A H -0.2491 1.0212 0.2080 0.092 Uiso 1 1 calc R . .
H24B H -0.2603 0.8571 0.1933 0.092 Uiso 1 1 calc R . .
H24C H -0.2131 0.9494 0.1305 0.092 Uiso 1 1 calc R . .
C25 C -0.0399(4) 0.9653(3) 0.30041(11) 0.0558(7) Uani 1 1 d . . .
H25A H 0.0589 0.9715 0.3192 0.084 Uiso 1 1 calc R . .
H25B H -0.0942 0.8828 0.3150 0.084 Uiso 1 1 calc R . .
H25C H -0.0767 1.0473 0.3210 0.084 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'
Mg Mg 0.0486 0.0363 '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_
_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 Si1 C13 115.45(8) . . ?
N1 Si1 C15 114.63(7) . . ?
C13 Si1 C15 105.68(9) . . ?
N1 Si1 C14 104.41(8) . . ?
C13 Si1 C14 107.63(11) . . ?
C15 Si1 C14 108.74(8) . . ?
N1 Si1 Mg1 34.93(4) . . ?
C13 Si1 Mg1 126.06(7) . . ?
C15 Si1 Mg1 126.79(6) . . ?
C14 Si1 Mg1 69.48(7) . . ?
N1 Mg1 N1 180.0 . 2_666 ?
N1 Mg1 Si1 30.68(4) . . ?
N1 Mg1 Si1 149.32(4) 2_666 . ?
N1 Mg1 Si1 149.32(4) . 2_666 ?
N1 Mg1 Si1 30.68(4) 2_666 2_666 ?
Si1 Mg1 Si1 180.0 . 2_666 ?
C1 N1 Si1 123.36(10) . . ?
C1 N1 Mg1 122.17(10) . . ?
Si1 N1 Mg1 114.38(7) . . ?
C6 C1 C2 119.15(13) . . ?
C6 C1 N1 120.54(13) . . ?
C2 C1 N1 120.26(13) . . ?
C3 C2 C1 119.33(14) . . ?
C3 C2 C7 119.75(14) . . ?
C1 C2 C7 120.90(13) . . ?
C5 C6 C1 119.45(14) . . ?
C5 C6 C8 119.30(14) . . ?
C1 C6 C8 121.20(13) . . ?
C4 C5 C6 121.38(15) . . ?
C2 C7 C10 113.48(14) . . ?
C2 C7 C9 111.16(15) . . ?
C10 C7 C9 109.77(15) . . ?
C4 C3 C2 121.21(15) . . ?
C6 C8 C12 113.20(13) . . ?
C6 C8 C11 110.85(14) . . ?
C12 C8 C11 110.02(14) . . ?
C3 C4 C5 119.48(15) . . ?
N2 Si2 C28 114.90(8) . . ?
N2 Si2 C30 114.27(7) . . ?
C28 Si2 C30 106.38(11) . . ?
N2 Si2 C29 103.37(7) . . ?
C28 Si2 C29 108.38(10) . . ?
C30 Si2 C29 109.33(8) . . ?
N2 Si2 Mg2 34.49(4) . . ?
C28 Si2 Mg2 122.36(8) . . ?
C30 Si2 Mg2 129.47(6) . . ?
C29 Si2 Mg2 69.09(6) . . ?
N2 Mg2 N2 180.00(8) 2_575 . ?
N2 Mg2 C16 26.38(5) 2_575 2_575 ?
N2 Mg2 C16 153.62(5) . 2_575 ?
N2 Mg2 C16 153.62(5) 2_575 . ?
N2 Mg2 C16 26.38(5) . . ?
C16 Mg2 C16 180.00(5) 2_575 . ?
N2 Mg2 Si2 30.39(4) 2_575 2_575 ?
N2 Mg2 Si2 149.61(4) . 2_575 ?
C16 Mg2 Si2 56.66(3) 2_575 2_575 ?
C16 Mg2 Si2 123.34(3) . 2_575 ?
N2 Mg2 Si2 149.61(4) 2_575 . ?
N2 Mg2 Si2 30.39(4) . . ?
C16 Mg2 Si2 123.34(3) 2_575 . ?
C16 Mg2 Si2 56.66(3) . . ?
Si2 Mg2 Si2 180.000(13) 2_575 . ?
C16 N2 Si2 127.42(10) . . ?
C16 N2 Mg2 117.04(10) . . ?
Si2 N2 Mg2 115.12(7) . . ?
C17 C16 C21 119.40(13) . . ?
C17 C16 N2 120.75(13) . . ?
C21 C16 N2 119.72(13) . . ?
C17 C16 Mg2 116.88(10) . . ?
C21 C16 Mg2 108.60(9) . . ?
N2 C16 Mg2 36.58(6) . . ?
C18 C17 C16 119.24(14) . . ?
C18 C17 C22 119.09(14) . . ?
C16 C17 C22 121.65(13) . . ?
C19 C20 C21 121.36(15) . . ?
C20 C21 C16 119.17(14) . . ?
C20 C21 C23 119.75(14) . . ?
C16 C21 C23 121.01(13) . . ?
C25 C22 C17 112.66(14) . . ?
C25 C22 C24 110.5(2) . . ?
C17 C22 C24 111.78(15) . . ?
C19 C18 C17 121.09(15) . . ?
C21 C23 C26 111.36(13) . . ?
C21 C23 C27 113.31(14) . . ?
C26 C23 C27 109.88(16) . . ?
C18 C19 C20 119.72(15) . . ?
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
Si1 N1 1.7138(13) . ?
Si1 C13 1.871(2) . ?
Si1 C15 1.8740(18) . ?
Si1 C14 1.8763(19) . ?
Si1 Mg1 3.0588(4) . ?
Mg1 N1 1.9229(12) . ?
Mg1 N1 1.9229(12) 2_666 ?
Mg1 Si1 3.0588(4) 2_666 ?
N1 C1 1.4275(18) . ?
C1 C6 1.416(2) . ?
C1 C2 1.422(2) . ?
C2 C3 1.398(2) . ?
C2 C7 1.522(2) . ?
C6 C5 1.394(2) . ?
C6 C8 1.527(2) . ?
C5 C4 1.388(2) . ?
C7 C10 1.530(2) . ?
C7 C9 1.532(3) . ?
C3 C4 1.387(2) . ?
C8 C12 1.530(2) . ?
C8 C11 1.530(2) . ?
Si2 N2 1.7103(13) . ?
Si2 C28 1.863(2) . ?
Si2 C30 1.8758(19) . ?
Si2 C29 1.8870(17) . ?
Si2 Mg2 3.0610(4) . ?
Mg2 N2 1.9142(12) 2_575 ?
Mg2 N2 1.9142(12) . ?
Mg2 C16 2.8612(14) 2_575 ?
Mg2 C16 2.8612(14) . ?
Mg2 Si2 3.0610(4) 2_575 ?
N2 C16 1.4275(19) . ?
C16 C17 1.418(2) . ?
C16 C21 1.420(2) . ?
C17 C18 1.401(2) . ?
C17 C22 1.520(2) . ?
C20 C19 1.387(2) . ?
C20 C21 1.395(2) . ?
C21 C23 1.524(2) . ?
C22 C25 1.517(3) . ?
C22 C24 1.522(3) . ?
C18 C19 1.384(2) . ?
C23 C26 1.528(2) . ?
C23 C27 1.528(2) . ?
