#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/30/7013017.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_7013017
loop_
_publ_author_name
'Dove, Andrew P.'
'Gibson, Vernon C.'
'Hormnirun, Pimpa'
'Marshall, Edward L.'
'Segal, John A.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Low coordinate magnesium chemistry supported by a bulky ?-diketiminate
 ligand
;
_journal_issue                   15
_journal_name_full               'Dalton Transactions'
_journal_page_first              3088
_journal_paper_doi               10.1039/b303550f
_journal_year                    2003
_chemical_formula_sum            'C35 H59 Mg N3 Si2'
_chemical_formula_weight         602.34
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.148(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1369(5)
_cell_length_b                   20.3728(7)
_cell_length_c                   20.235(3)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      11.13
_cell_volume                     3766.6(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5987
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.08
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.53
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0045(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.071
_refine_ls_goodness_of_fit_obs   1.099
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.099
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_obs          0.0400
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0602P)²+1.2948P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1113
_refine_ls_wR_factor_obs         0.1042
_reflns_number_observed          4786
_reflns_number_total             5590
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b303550f.txt
_cod_data_source_block           Compound_13
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+1.2948P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+1.2948P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3766.5(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C35 H59 N3 Si2 Mg'
_cod_database_code               7013017
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mg Mg 0.31107(6) 0.25477(3) 0.87245(3) 0.0218(2) Uani 1 d . .
C1 C 0.5255(2) 0.20523(9) 0.96764(9) 0.0238(4) Uani 1 d . .
N1 N 0.4054(2) 0.18911(7) 0.93346(7) 0.0215(3) Uani 1 d . .
C2 C 0.5741(2) 0.26948(9) 0.97772(9) 0.0259(4) Uani 1 d . .
H2A H 0.6668(2) 0.27324(9) 0.99878(9) 0.031 Uiso 1 calc R .
C3 C 0.5066(2) 0.32963(9) 0.96141(9) 0.0241(4) Uani 1 d . .
N3 N 0.3976(2) 0.33524(7) 0.91848(7) 0.0217(3) Uani 1 d . .
C4 C 0.6176(2) 0.15170(10) 0.99893(10) 0.0315(5) Uani 1 d . .
H4A H 0.6876(11) 0.17139(12) 1.0299(6) 0.047 Uiso 1 calc R .
H4B H 0.6708(13) 0.1279(5) 0.96440(12) 0.047 Uiso 1 calc R .
H4C H 0.5539(3) 0.1211(4) 1.0228(6) 0.047 Uiso 1 calc R .
C5 C 0.5648(2) 0.38868(10) 0.99842(11) 0.0345(5) Uani 1 d . .
H5A H 0.6542(10) 0.4044(5) 0.9770(5) 0.052 Uiso 1 calc R .
H5B H 0.5869(16) 0.3762(2) 1.0442(2) 0.052 Uiso 1 calc R .
H5C H 0.4911(7) 0.4236(3) 0.9981(7) 0.052 Uiso 1 calc R .
C6 C 0.3490(2) 0.12353(9) 0.94015(9) 0.0254(4) Uani 1 d . .
C7 C 0.3921(2) 0.07365(10) 0.89644(10) 0.0324(5) Uani 1 d . .
C8 C 0.3284(3) 0.01201(11) 0.90292(13) 0.0446(6) Uani 1 d . .
H8A H 0.3555(3) -0.02215(11) 0.87344(13) 0.053 Uiso 1 calc R .
C9 C 0.2271(3) -0.00022(11) 0.95114(14) 0.0491(6) Uani 1 d . .
H9A H 0.1850(3) -0.04270(11) 0.95486(14) 0.059 Uiso 1 calc R .
C10 C 0.1859(2) 0.04859(11) 0.99423(12) 0.0417(6) Uani 1 d . .
H10A H 0.1159(2) 0.03922(11) 1.02756(12) 0.050 Uiso 1 calc R .
C11 C 0.2448(2) 0.11148(10) 0.98991(10) 0.0288(4) Uani 1 d . .
C12 C 0.5044(3) 0.08501(11) 0.84231(11) 0.0417(5) Uani 1 d . .
H12A H 0.5454(3) 0.13013(11) 0.84826(11) 0.050 Uiso 1 calc R .
C13 C 0.4320(4) 0.08200(15) 0.77419(13) 0.0675(9) Uani 1 d . .
H13A H 0.5060(4) 0.08942(15) 0.73999(13) 0.101 Uiso 1 calc R .
H13B H 0.3563(4) 0.11594(15) 0.77107(13) 0.101 Uiso 1 calc R .
H13C H 0.3874(4) 0.03870(15) 0.76783(13) 0.101 Uiso 1 calc R .
C14 C 0.6314(3) 0.03626(15) 0.8460(2) 0.0664(8) Uani 1 d . .
H14A H 0.7009(3) 0.04539(15) 0.8103(2) 0.100 Uiso 1 calc R .
H14B H 0.5937(3) -0.00853(15) 0.8413(2) 0.100 Uiso 1 calc R .
H14C H 0.6812(3) 0.04070(15) 0.8888(2) 0.100 Uiso 1 calc R .
C15 C 0.1983(2) 0.16502(11) 1.03779(11) 0.0337(5) Uani 1 d . .
H15A H 0.2073(2) 0.20787(11) 1.01404(11) 0.040 Uiso 1 calc R .
C16 C 0.2975(3) 0.16849(14) 1.09837(12) 0.0530(7) Uani 1 d . .
H16A H 0.2636(3) 0.20354(14) 1.12775(12) 0.079 Uiso 1 calc R .
H16B H 0.3980(3) 0.17770(14) 1.08442(12) 0.079 Uiso 1 calc R .
H16C H 0.2946(3) 0.12645(14) 1.12188(12) 0.079 Uiso 1 calc R .
C17 C 0.0394(2) 0.15875(14) 1.06045(13) 0.0491(6) Uani 1 d . .
H17A H 0.0163(2) 0.19453(14) 1.09107(13) 0.074 Uiso 1 calc R .
H17B H 0.0258(2) 0.11653(14) 1.08281(13) 0.074 Uiso 1 calc R .
H17C H -0.0258(2) 0.16118(14) 1.02199(13) 0.074 Uiso 1 calc R .
C18 C 0.3300(2) 0.39800(9) 0.90780(9) 0.0243(4) Uani 1 d . .
C19 C 0.1893(2) 0.40823(10) 0.93518(10) 0.0278(4) Uani 1 d . .
C20 C 0.1182(2) 0.46705(11) 0.92199(11) 0.0378(5) Uani 1 d . .
H20A H 0.0236(2) 0.47443(11) 0.93980(11) 0.045 Uiso 1 calc R .
C21 C 0.1822(3) 0.51492(11) 0.88360(11) 0.0425(6) Uani 1 d . .
H21A H 0.1317(3) 0.55481(11) 0.87510(11) 0.051 Uiso 1 calc R .
C22 C 0.3193(3) 0.50482(10) 0.85761(11) 0.0390(5) Uani 1 d . .
H22A H 0.3627(3) 0.53827(10) 0.83149(11) 0.047 Uiso 1 calc R .
C23 C 0.3962(2) 0.44672(10) 0.86864(10) 0.0299(4) Uani 1 d . .
C24 C 0.1207(2) 0.35657(10) 0.97990(10) 0.0320(5) Uani 1 d . .
H24A H 0.1482(2) 0.31260(10) 0.96181(10) 0.038 Uiso 1 calc R .
C25 C -0.0465(2) 0.35954(13) 0.98194(13) 0.0455(6) Uani 1 d . .
H25A H -0.0834(2) 0.32520(13) 1.01144(13) 0.068 Uiso 1 calc R .
H25B H -0.0858(2) 0.35272(13) 0.93736(13) 0.068 Uiso 1 calc R .
H25C H -0.0774(2) 0.40262(13) 0.99834(13) 0.068 Uiso 1 calc R .
C26 C 0.1810(3) 0.36046(13) 1.05019(11) 0.0468(6) Uani 1 d . .
H26A H 0.1346(3) 0.32666(13) 1.07750(11) 0.070 Uiso 1 calc R .
H26B H 0.1601(3) 0.40388(13) 1.06873(11) 0.070 Uiso 1 calc R .
H26C H 0.2871(3) 0.35332(13) 1.04947(11) 0.070 Uiso 1 calc R .
C27 C 0.5475(2) 0.43959(10) 0.83785(11) 0.0354(5) Uani 1 d . .
H27A H 0.5872(2) 0.39558(10) 0.85050(11) 0.042 Uiso 1 calc R .
C28 C 0.6546(3) 0.49205(13) 0.86305(14) 0.0532(7) Uani 1 d . .
H28A H 0.7502(3) 0.48575(13) 0.84213(14) 0.080 Uiso 1 calc R .
H28B H 0.6651(3) 0.48815(13) 0.91110(14) 0.080 Uiso 1 calc R .
H28C H 0.6169(3) 0.53574(13) 0.85200(14) 0.080 Uiso 1 calc R .
C29 C 0.5417(3) 0.44311(13) 0.76202(12) 0.0495(6) Uani 1 d . .
H29A H 0.6408(3) 0.43835(13) 0.74419(12) 0.074 Uiso 1 calc R .
H29B H 0.5011(3) 0.48556(13) 0.74844(12) 0.074 Uiso 1 calc R .
H29C H 0.4795(3) 0.40768(13) 0.74508(12) 0.074 Uiso 1 calc R .
N30 N 0.1769(2) 0.24697(8) 0.79702(8) 0.0249(4) Uani 1 d . .
Si31 Si -0.00628(6) 0.23349(3) 0.80326(3) 0.0352(2) Uani 1 d . .
C32 C -0.1150(3) 0.3110(2) 0.79527(14) 0.0634(8) Uani 1 d . .
H32A H -0.0955(3) 0.3312(2) 0.75222(14) 0.095 Uiso 1 calc R .
H32B H -0.0869(3) 0.3415(2) 0.83054(14) 0.095 Uiso 1 calc R .
H32C H -0.2195(3) 0.3008(2) 0.79885(14) 0.095 Uiso 1 calc R .
C33 C -0.0470(3) 0.19704(14) 0.88570(13) 0.0524(6) Uani 1 d . .
H33A H -0.0097(3) 0.22606(14) 0.92052(13) 0.079 Uiso 1 calc R .
H33B H 0.0004(3) 0.15404(14) 0.88930(13) 0.079 Uiso 1 calc R .
H33C H -0.1530(3) 0.19187(14) 0.89063(13) 0.079 Uiso 1 calc R .
C34 C -0.0804(3) 0.1755(2) 0.7399(2) 0.0719(9) Uani 1 d . .
H34A H -0.0612(3) 0.1929(2) 0.6956(2) 0.108 Uiso 1 calc R .
H34B H -0.1862(3) 0.1705(2) 0.7461(2) 0.108 Uiso 1 calc R .
H34C H -0.0327(3) 0.1327(2) 0.7448(2) 0.108 Uiso 1 calc R .
Si35 Si 0.26825(6) 0.26859(3) 0.72726(3) 0.0277(2) Uani 1 d . .
C36 C 0.4688(2) 0.26891(11) 0.74981(11) 0.0359(5) Uani 1 d . .
H36A H 0.4851(2) 0.29879(11) 0.78706(11) 0.054 Uiso 1 calc R .
H36B H 0.5263(2) 0.28363(11) 0.71177(11) 0.054 Uiso 1 calc R .
H36C H 0.4992(2) 0.22446(11) 0.76229(11) 0.054 Uiso 1 calc R .
C37 C 0.2138(3) 0.35146(12) 0.69531(12) 0.0450(6) Uani 1 d . .
H37A H 0.2225(3) 0.38390(12) 0.73086(12) 0.068 Uiso 1 calc R .
H37B H 0.1123(3) 0.34995(12) 0.67967(12) 0.068 Uiso 1 calc R .
H37C H 0.2781(3) 0.36385(12) 0.65871(12) 0.068 Uiso 1 calc R .
C38 C 0.2479(3) 0.21052(13) 0.65611(11) 0.0485(6) Uani 1 d . .
H38A H 0.2752(3) 0.16617(13) 0.67027(11) 0.073 Uiso 1 calc R .
H38B H 0.3119(3) 0.22445(13) 0.61993(11) 0.073 Uiso 1 calc R .
H38C H 0.1460(3) 0.21055(13) 0.64090(11) 0.073 Uiso 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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
N30 Mg N1 133.57(7) . . ?
N30 Mg N3 131.28(7) . . ?
N1 Mg N3 95.11(6) . . ?
N1 C1 C2 124.5(2) . . ?
N1 C1 C4 119.6(2) . . ?
C2 C1 C4 116.0(2) . . ?
C1 N1 C6 118.24(15) . . ?
C1 N1 Mg 120.25(12) . . ?
C6 N1 Mg 121.48(12) . . ?
C1 C2 C3 129.9(2) . . ?
N3 C3 C2 123.8(2) . . ?
N3 C3 C5 121.3(2) . . ?
C2 C3 C5 114.9(2) . . ?
C3 N3 C18 119.85(15) . . ?
C3 N3 Mg 121.26(12) . . ?
C18 N3 Mg 118.68(11) . . ?
C7 C6 C11 121.0(2) . . ?
C7 C6 N1 120.8(2) . . ?
C11 C6 N1 118.1(2) . . ?
C8 C7 C6 118.4(2) . . ?
C8 C7 C12 119.3(2) . . ?
C6 C7 C12 122.3(2) . . ?
C9 C8 C7 121.0(2) . . ?
C8 C9 C10 120.4(2) . . ?
C9 C10 C11 121.2(2) . . ?
C10 C11 C6 117.8(2) . . ?
C10 C11 C15 120.8(2) . . ?
C6 C11 C15 121.4(2) . . ?
C7 C12 C13 110.6(2) . . ?
C7 C12 C14 112.3(2) . . ?
C13 C12 C14 110.2(2) . . ?
C11 C15 C16 112.3(2) . . ?
C11 C15 C17 113.5(2) . . ?
C16 C15 C17 109.0(2) . . ?
C23 C18 C19 120.5(2) . . ?
C23 C18 N3 121.8(2) . . ?
C19 C18 N3 117.6(2) . . ?
C20 C19 C18 118.4(2) . . ?
C20 C19 C24 121.1(2) . . ?
C18 C19 C24 120.4(2) . . ?
C21 C20 C19 121.3(2) . . ?
C22 C21 C20 119.8(2) . . ?
C21 C22 C23 121.7(2) . . ?
C22 C23 C18 118.1(2) . . ?
C22 C23 C27 118.2(2) . . ?
C18 C23 C27 123.7(2) . . ?
C19 C24 C26 111.7(2) . . ?
C19 C24 C25 113.7(2) . . ?
C26 C24 C25 109.3(2) . . ?
C23 C27 C28 112.1(2) . . ?
C23 C27 C29 112.0(2) . . ?
C28 C27 C29 108.6(2) . . ?
Si35 N30 Si31 126.05(9) . . ?
Si35 N30 Mg 108.56(8) . . ?
Si31 N30 Mg 124.63(9) . . ?
N30 Si31 C33 109.22(10) . . ?
N30 Si31 C34 113.95(11) . . ?
C33 Si31 C34 106.80(14) . . ?
N30 Si31 C32 112.30(12) . . ?
C33 Si31 C32 107.83(13) . . ?
C34 Si31 C32 106.4(2) . . ?
N30 Si35 C38 115.28(10) . . ?
N30 Si35 C37 112.92(10) . . ?
C38 Si35 C37 106.16(12) . . ?
N30 Si35 C36 106.17(9) . . ?
C38 Si35 C36 106.39(11) . . ?
C37 Si35 C36 109.69(10) . . ?
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
Mg N30 1.961(2) . ?
Mg N1 2.013(2) . ?
Mg N3 2.044(2) . ?
C1 N1 1.337(2) . ?
C1 C2 1.397(3) . ?
C1 C4 1.515(3) . ?
N1 C6 1.438(2) . ?
C2 C3 1.411(3) . ?
C3 N3 1.325(2) . ?
C3 C5 1.513(3) . ?
N3 C18 1.436(2) . ?
C6 C7 1.404(3) . ?
C6 C11 1.409(3) . ?
C7 C8 1.391(3) . ?
C7 C12 1.520(3) . ?
C8 C9 1.369(4) . ?
C9 C10 1.376(4) . ?
C10 C11 1.392(3) . ?
C11 C15 1.520(3) . ?
C12 C13 1.528(3) . ?
C12 C14 1.529(3) . ?
C15 C16 1.524(3) . ?
C15 C17 1.529(3) . ?
C18 C23 1.408(3) . ?
C18 C19 1.416(3) . ?
C19 C20 1.389(3) . ?
C19 C24 1.524(3) . ?
C20 C21 1.378(3) . ?
C21 C22 1.375(3) . ?
C22 C23 1.394(3) . ?
C23 C27 1.525(3) . ?
C24 C26 1.526(3) . ?
C24 C25 1.530(3) . ?
C27 C28 1.535(3) . ?
C27 C29 1.537(3) . ?
N30 Si35 1.700(2) . ?
N30 Si31 1.701(2) . ?
Si31 C33 1.864(3) . ?
Si31 C34 1.869(3) . ?
Si31 C32 1.872(3) . ?
Si35 C38 1.872(2) . ?
Si35 C37 1.874(2) . ?
Si35 C36 1.888(2) . ?
