#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179469 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/66/4336606.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_4336606
loop_
_publ_author_name
'Andrés Garcés'
'Luis F. Sánchez-Barba'
'Juan Fernández-Baeza'
'Antonio Otero'
'Manuel Honrado'
'Agustín Lara-Sánchez'
'Ana M. Rodríguez'
_publ_contact_author
;                                                                               
     'Sánchez-Barba, LF.'                                     
      Departamento de Química Inorgánica y Analítica 
      Universidad Rey Juan Carlos
      Mostoles
      28933-Madrid
      Spain.
;
_publ_contact_author_email       luisfernando.sanchezbarba@urjc.es
_publ_contact_author_phone       '+34 926295300'
_publ_section_title
;
 Heteroscorpionate Magnesium Alkyls Bearing Unprecedented Apical
 σ-C(sp3)-Mg Bonds: Heteroselective Ring-Opening Polymerization of
 rac-Lactide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12691
_journal_page_last               12701
_journal_paper_doi               10.1021/ic401915b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C25 H36 Mg N6'
_chemical_formula_sum            'C25 H36 Mg N6'
_chemical_formula_weight         444.91
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.45(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.238(4)
_cell_length_b                   14.626(3)
_cell_length_c                   15.190(6)
_cell_measurement_reflns_used    608
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      14.915
_cell_measurement_theta_min      2.288
_cell_volume                     2696.0(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'WINGX v1.70 (Farrugia, 1999)'
_computing_publication_material  'WINGX v1.70 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      260(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.1111
_diffrn_reflns_av_sigmaI/netI    0.1391
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13233
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.9784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1791
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0708P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1847
_reflns_number_gt                1980
_reflns_number_total             4620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401915b_si_001_2.cif
_cod_data_source_block           4
_cod_original_cell_volume        2695.9(15)
_cod_database_code               4336606
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mg1 Mg 0.40883(11) 0.28811(9) 0.11545(9) 0.0467(4) Uani 1 1 d .
N1 N 0.3690(3) 0.1719(2) 0.0289(2) 0.0469(9) Uani 1 1 d .
N2 N 0.4488(3) 0.1579(2) -0.0267(2) 0.0430(9) Uani 1 1 d .
N3 N 0.4237(3) 0.3631(2) -0.0043(2) 0.0447(9) Uani 1 1 d .
N4 N 0.4867(3) 0.3155(2) -0.0594(2) 0.0430(9) Uani 1 1 d .
N5 N 0.5753(3) 0.2556(2) 0.1301(2) 0.0479(9) Uani 1 1 d .
N6 N 0.7241(3) 0.2112(2) 0.0544(2) 0.0548(10) Uani 1 1 d .
C1 C 0.4278(4) 0.0805(2) -0.0781(3) 0.0426(11) Uani 1 1 d .
C2 C 0.3323(4) 0.0439(3) -0.0531(3) 0.0516(12) Uani 1 1 d .
H2 H 0.2974 -0.0095 -0.0749 0.062 Uiso 1 1 calc R
C3 C 0.2979(3) 0.1021(3) 0.0110(3) 0.0462(11) Uani 1 1 d .
C4 C 0.4993(3) 0.0482(3) -0.1450(3) 0.0569(13) Uani 1 1 d .
H4A H 0.4843 0.0841 -0.1981 0.085 Uiso 1 1 calc R
H4B H 0.4839 -0.0149 -0.1586 0.085 Uiso 1 1 calc R
H4C H 0.5754 0.0549 -0.1210 0.085 Uiso 1 1 calc R
C5 C 0.1973(4) 0.0948(3) 0.0576(3) 0.0680(14) Uani 1 1 d .
H5A H 0.1656 0.0351 0.0480 0.102 Uiso 1 1 calc R
H5B H 0.1444 0.1402 0.0345 0.102 Uiso 1 1 calc R
H5C H 0.2175 0.1047 0.1201 0.102 Uiso 1 1 calc R
C6 C 0.4894(3) 0.3609(3) -0.1379(3) 0.0462(11) Uani 1 1 d .
C7 C 0.4275(4) 0.4393(3) -0.1326(3) 0.0516(12) Uani 1 1 d .
H7 H 0.4150 0.4843 -0.1760 0.062 Uiso 1 1 calc R
C8 C 0.3870(3) 0.4390(3) -0.0504(3) 0.0441(11) Uani 1 1 d .
C9 C 0.5459(4) 0.3233(3) -0.2122(3) 0.0670(14) Uani 1 1 d .
H9A H 0.5361 0.3646 -0.2616 0.100 Uiso 1 1 calc R
H9B H 0.5147 0.2649 -0.2301 0.100 Uiso 1 1 calc R
H9C H 0.6232 0.3162 -0.1922 0.100 Uiso 1 1 calc R
C10 C 0.3109(4) 0.5049(3) -0.0132(3) 0.0599(13) Uani 1 1 d .
H10A H 0.2359 0.4880 -0.0329 0.090 Uiso 1 1 calc R
H10B H 0.3242 0.5655 -0.0334 0.090 Uiso 1 1 calc R
H10C H 0.3238 0.5032 0.0505 0.090 Uiso 1 1 calc R
C11 C 0.5366(3) 0.2272(2) -0.0306(3) 0.0416(11) Uani 1 1 d .
H11 H 0.5785 0.2074 -0.0779 0.050 Uiso 1 1 calc R
C12 C 0.6209(4) 0.2311(3) 0.0564(3) 0.0452(11) Uani 1 1 d .
C13 C 0.7692(3) 0.1912(3) -0.0291(3) 0.0660(14) Uani 1 1 d .
H13A H 0.7547 0.2421 -0.0699 0.079 Uiso 1 1 calc R
H13B H 0.7340 0.1371 -0.0568 0.079 Uiso 1 1 calc R
C14 C 0.8920(4) 0.1756(4) -0.0088(4) 0.0944(18) Uani 1 1 d .
H14A H 0.9274 0.2315 0.0122 0.142 Uiso 1 1 calc R
H14B H 0.9205 0.1563 -0.0618 0.142 Uiso 1 1 calc R
H14C H 0.9061 0.1293 0.0359 0.142 Uiso 1 1 calc R
C15 C 0.6485(3) 0.2577(3) 0.2169(3) 0.0488(11) Uani 1 1 d .
C16 C 0.6923(4) 0.1617(3) 0.2459(3) 0.0749(16) Uani 1 1 d .
H16A H 0.6314 0.1210 0.2488 0.112 Uiso 1 1 calc R
H16B H 0.7354 0.1656 0.3033 0.112 Uiso 1 1 calc R
H16C H 0.7375 0.1389 0.2036 0.112 Uiso 1 1 calc R
C17 C 0.7468(4) 0.3251(3) 0.2188(3) 0.0660(14) Uani 1 1 d .
H17A H 0.7951 0.3048 0.1778 0.099 Uiso 1 1 calc R
H17B H 0.7864 0.3271 0.2776 0.099 Uiso 1 1 calc R
H17C H 0.7195 0.3850 0.2022 0.099 Uiso 1 1 calc R
C18 C 0.5776(4) 0.2904(3) 0.2878(3) 0.0733(15) Uani 1 1 d .
H18A H 0.5498 0.3506 0.2728 0.110 Uiso 1 1 calc R
H18B H 0.6218 0.2919 0.3448 0.110 Uiso 1 1 calc R
H18C H 0.5170 0.2491 0.2898 0.110 Uiso 1 1 calc R
C19 C 0.2932(4) 0.3186(3) 0.2077(3) 0.0670(14) Uani 1 1 d .
H19A H 0.2563 0.2620 0.2194 0.080 Uiso 1 1 calc R
H19B H 0.3354 0.3375 0.2632 0.080 Uiso 1 1 calc R
C20 C 0.2062(4) 0.3894(3) 0.1831(3) 0.0519(12) Uani 1 1 d .
C21 C 0.1065(4) 0.3696(3) 0.1310(3) 0.0591(13) Uani 1 1 d .
H21 H 0.0919 0.3096 0.1129 0.071 Uiso 1 1 calc R
C22 C 0.0288(4) 0.4365(4) 0.1053(3) 0.0772(16) Uani 1 1 d .
H22 H -0.0362 0.4205 0.0700 0.093 Uiso 1 1 calc R
C23 C 0.0455(6) 0.5262(4) 0.1310(4) 0.0896(19) Uani 1 1 d .
H23 H -0.0075 0.5706 0.1140 0.107 Uiso 1 1 calc R
C24 C 0.1427(6) 0.5485(4) 0.1823(4) 0.0901(19) Uani 1 1 d .
H24 H 0.1559 0.6087 0.2002 0.108 Uiso 1 1 calc R
C25 C 0.2217(5) 0.4817(4) 0.2078(3) 0.0780(16) Uani 1 1 d .
H25 H 0.2869 0.4986 0.2423 0.094 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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N5 Mg1 N3 91.03(15)
N5 Mg1 C19 133.87(17)
N3 Mg1 C19 125.22(16)
N5 Mg1 N1 91.49(14)
N3 Mg1 N1 85.63(13)
C19 Mg1 N1 116.13(17)
C3 N1 N2 104.7(3)
C3 N1 Mg1 143.8(3)
N2 N1 Mg1 111.4(2)
C1 N2 N1 111.8(3)
C1 N2 C11 128.3(4)
N1 N2 C11 119.6(3)
C8 N3 N4 105.7(3)
C8 N3 Mg1 142.6(3)
N4 N3 Mg1 111.5(2)
C6 N4 N3 111.0(3)
C6 N4 C11 129.0(3)
N3 N4 C11 120.0(3)
C12 N5 C15 117.9(3)
C12 N5 Mg1 118.2(3)
C15 N5 Mg1 123.9(3)
C12 N6 C13 122.5(4)
N2 C1 C2 105.3(4)
N2 C1 C4 124.0(4)
C2 C1 C4 130.7(4)
C1 C2 C3 107.3(4)
N1 C3 C2 110.9(4)
N1 C3 C5 120.4(4)
C2 C3 C5 128.6(4)
N4 C6 C7 106.0(4)
N4 C6 C9 122.8(4)
C7 C6 C9 131.1(4)
C6 C7 C8 108.0(4)
N3 C8 C7 109.3(4)
N3 C8 C10 120.7(4)
C7 C8 C10 129.9(4)
N4 C11 N2 109.7(3)
N4 C11 C12 114.9(3)
N2 C11 C12 113.0(3)
N6 C12 N5 125.5(4)
N6 C12 C11 120.5(4)
N5 C12 C11 114.0(4)
N6 C13 C14 109.1(4)
N5 C15 C18 107.1(3)
N5 C15 C16 112.3(3)
C18 C15 C16 106.8(4)
N5 C15 C17 113.8(3)
C18 C15 C17 107.1(4)
C16 C15 C17 109.4(3)
C20 C19 Mg1 119.0(3)
C21 C20 C25 115.3(4)
C21 C20 C19 122.6(4)
C25 C20 C19 122.0(5)
C22 C21 C20 122.1(5)
C23 C22 C21 121.5(5)
C24 C23 C22 118.2(5)
C23 C24 C25 120.6(5)
C24 C25 C20 122.3(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mg1 N5 2.075(4)
Mg1 N3 2.152(4)
Mg1 C19 2.163(5)
Mg1 N1 2.165(3)
N1 C3 1.346(5)
N1 N2 1.387(4)
N2 C1 1.381(4)
N2 C11 1.484(5)
N3 C8 1.357(5)
N3 N4 1.395(4)
N4 C6 1.370(5)
N4 C11 1.470(4)
N5 C12 1.362(5)
N5 C15 1.495(5)
N6 C12 1.300(5)
N6 C13 1.476(5)
C1 C2 1.383(5)
C1 C4 1.500(5)
C2 C3 1.399(6)
C3 C5 1.501(6)
C6 C7 1.383(5)
C6 C9 1.501(6)
C7 C8 1.403(6)
C8 C10 1.500(5)
C11 C12 1.569(5)
C13 C14 1.512(6)
C15 C18 1.544(6)
C15 C16 1.547(5)
C15 C17 1.552(6)
C19 C20 1.497(5)
C20 C21 1.395(6)
C20 C25 1.408(6)
C21 C22 1.386(6)
C22 C23 1.376(7)
C23 C24 1.374(7)
C24 C25 1.393(7)
