#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:06:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179231 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/51/4315171.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_4315171
loop_
_publ_author_name
'Andrés Garcés'
'Luis F. Sánchez-Barba'
'Carlos Alonso-Moreno'
'Mariano Fajardo'
'Juan Fernández-Baeza'
'Antonio Otero'
'Agustín Lara-Sánchez'
'Isabel López-Solera'
'Ana María Rodríguez'
_publ_contact_author
;
Isabel López-Solera
Departamento de Química Inórganica, Orgánica y Bioquímica
Facultad de Químicas
Universidad Castilla La Mancha
13071-Ciudad Real 
Spain
;
_publ_contact_author_email       Mabel.Lopez@uclm.es
_publ_contact_author_fax         '+34 926 295318'
_publ_contact_author_phone       '+34 926 295300 (ext:6282)'
_publ_section_title
;
 Hybrid Scorpionate/Cyclopentadienyl Magnesium and Zinc Complexes:
 Synthesis, Coordination Chemistry, and Ring-Opening Polymerization
 Studies on Cyclic Esters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2859
_journal_page_last               2871
_journal_paper_doi               10.1021/ic902399r
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C33 H40 Mg N4 Si'
_chemical_formula_weight         545.09
_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                114.121(18)
_cell_angle_beta                 96.94(3)
_cell_angle_gamma                90.904(15)
_cell_formula_units_Z            2
_cell_length_a                   9.063(10)
_cell_length_b                   13.584(19)
_cell_length_c                   13.952(19)
_cell_measurement_temperature    180(2)
_cell_volume                     1552(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_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      180(2)
_diffrn_measured_fraction_theta_full 0.252
_diffrn_measured_fraction_theta_max 0.252
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1454
_diffrn_reflns_av_sigmaI/netI    0.1609
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            7900
_diffrn_reflns_theta_full        29.03
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.017165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         2085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          1.130
_refine_ls_shift/su_mean         0.054
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0777P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.2099
_reflns_number_gt                981
_reflns_number_total             2085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902399r_si_001_3.cif
_cod_data_source_block           5
_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               4315171
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
Mg1 Mg 0.2392(3) 0.2825(3) 1.0445(3) 0.0454(13) Uani 1 1 d . . .
Si1 Si 0.2745(3) 0.3479(3) 1.3180(2) 0.0519(12) Uani 1 1 d . . .
N1 N 0.0369(8) 0.1818(7) 0.9484(8) 0.040(3) Uani 1 1 d . . .
N2 N -0.0036(11) 0.1696(8) 0.8456(8) 0.043(3) Uani 1 1 d . . .
N3 N 0.1766(8) 0.3788(9) 0.9516(7) 0.042(3) Uani 1 1 d . . .
N4 N 0.1225(9) 0.3237(8) 0.8432(9) 0.041(3) Uani 1 1 d . . .
C1 C 0.2593(11) 0.1486(10) 0.7833(10) 0.034(4) Uani 1 1 d . . .
C2 C 0.1043(10) 0.2067(10) 0.7913(9) 0.048(4) Uani 1 1 d . . .
H2 H 0.0564 0.1875 0.7185 0.057 Uiso 1 1 calc R . .
C3 C -0.0854(14) 0.1494(9) 0.9767(10) 0.039(4) Uani 1 1 d . . .
C4 C -0.2028(13) 0.1236(9) 0.8937(10) 0.052(4) Uani 1 1 d . . .
H4 H -0.3004 0.1026 0.8950 0.063 Uiso 1 1 calc R . .
C5 C -0.1513(14) 0.1343(9) 0.8116(11) 0.051(5) Uani 1 1 d . . .
C6 C -0.0847(12) 0.1508(11) 1.0838(8) 0.077(5) Uani 1 1 d . . .
H6A H -0.0575 0.0822 1.0822 0.116 Uiso 1 1 calc R . .
H6B H -0.1823 0.1642 1.1045 0.116 Uiso 1 1 calc R . .
H6C H -0.0140 0.2069 1.1339 0.116 Uiso 1 1 calc R . .
C7 C -0.2316(13) 0.1275(10) 0.7087(9) 0.068(4) Uani 1 1 d . . .
H7A H -0.3360 0.1105 0.7048 0.102 Uiso 1 1 calc R . .
H7B H -0.1927 0.0719 0.6510 0.102 Uiso 1 1 calc R . .
H7C H -0.2175 0.1956 0.7043 0.102 Uiso 1 1 calc R . .
C8 C 0.1854(10) 0.4863(10) 0.9698(10) 0.041(4) Uani 1 1 d . . .
C9 C 0.1373(10) 0.4975(10) 0.8761(11) 0.045(3) Uani 1 1 d . . .
H9 H 0.1327 0.5615 0.8670 0.054 Uiso 1 1 calc R . .
C10 C 0.0975(11) 0.3933(13) 0.7992(9) 0.041(4) Uani 1 1 d . . .
C11 C 0.2376(12) 0.5691(8) 1.0778(8) 0.057(4) Uani 1 1 d . . .
H11A H 0.1724 0.5652 1.1257 0.085 Uiso 1 1 calc R . .
H11B H 0.2374 0.6396 1.0774 0.085 Uiso 1 1 calc R . .
H11C H 0.3369 0.5564 1.1006 0.085 Uiso 1 1 calc R . .
C12 C 0.0397(13) 0.3609(10) 0.6826(8) 0.066(4) Uani 1 1 d . . .
H12A H 0.1130 0.3223 0.6400 0.099 Uiso 1 1 calc R . .
H12B H 0.0204 0.4247 0.6708 0.099 Uiso 1 1 calc R . .
H12C H -0.0508 0.3155 0.6635 0.099 Uiso 1 1 calc R . .
C13 C 0.1992(10) 0.3766(8) 1.2043(6) 0.046(3) Uani 1 1 d . . .
H13A H 0.2334 0.4507 1.2213 0.056 Uiso 1 1 calc R . .
H13B H 0.0919 0.3755 1.2026 0.056 Uiso 1 1 calc R . .
C14 C 0.4776(11) 0.3974(9) 1.3536(7) 0.060(4) Uani 1 1 d . . .
H14A H 0.5279 0.3633 1.2928 0.090 Uiso 1 1 calc R . .
H14B H 0.5218 0.3797 1.4101 0.090 Uiso 1 1 calc R . .
H14C H 0.4866 0.4744 1.3761 0.090 Uiso 1 1 calc R . .
C15 C 0.1830(11) 0.4211(9) 1.4408(7) 0.070(5) Uani 1 1 d . . .
H15A H 0.1879 0.4972 1.4579 0.105 Uiso 1 1 calc R . .
H15B H 0.2342 0.4091 1.4991 0.105 Uiso 1 1 calc R . .
H15C H 0.0807 0.3941 1.4278 0.105 Uiso 1 1 calc R . .
C16 C 0.2545(11) 0.1998(9) 1.2904(8) 0.066(4) Uani 1 1 d . . .
H16A H 0.1508 0.1756 1.2745 0.100 Uiso 1 1 calc R . .
H16B H 0.2982 0.1898 1.3517 0.100 Uiso 1 1 calc R . .
H16C H 0.3043 0.1588 1.2311 0.100 Uiso 1 1 calc R . .
C21 C 0.3554(12) 0.1722(10) 0.8902(9) 0.032(3) Uani 1 1 d . . .
C22 C 0.3507(13) 0.1088(10) 0.9513(10) 0.052(4) Uani 1 1 d . . .
H22 H 0.3008 0.0365 0.9265 0.062 Uiso 1 1 calc R . .
C23 C 0.4501(13) 0.1611(10) 1.0451(10) 0.048(4) Uani 1 1 d . . .
H23 H 0.4768 0.1330 1.0989 0.057 Uiso 1 1 calc R . .
C24 C 0.5150(11) 0.2549(9) 1.0445(11) 0.040(4) Uani 1 1 d . . .
H24 H 0.5954 0.3028 1.0973 0.049 Uiso 1 1 calc R . .
C25 C 0.4599(14) 0.2617(11) 0.9527(11) 0.051(4) Uani 1 1 d . . .
H25 H 0.4976 0.3141 0.9282 0.061 Uiso 1 1 calc R . .
C31 C 0.3419(10) 0.1916(13) 0.7112(9) 0.049(4) Uani 1 1 d . . .
C32 C 0.3973(11) 0.2993(12) 0.7460(9) 0.049(4) Uani 1 1 d . . .
H32 H 0.3844 0.3498 0.8130 0.059 Uiso 1 1 calc R . .
C33 C 0.4706(11) 0.3302(11) 0.6811(9) 0.058(5) Uani 1 1 d . . .
H33 H 0.5096 0.4014 0.7064 0.070 Uiso 1 1 calc R . .
C34 C 0.4885(12) 0.2587(13) 0.5791(10) 0.069(5) Uani 1 1 d . . .
H34 H 0.5373 0.2818 0.5361 0.083 Uiso 1 1 calc R . .
C35 C 0.4320(12) 0.1521(11) 0.5424(9) 0.058(4) Uani 1 1 d . . .
H35 H 0.4436 0.1027 0.4745 0.069 Uiso 1 1 calc R . .
C36 C 0.3590(10) 0.1195(12) 0.6062(9) 0.065(5) Uani 1 1 d . . .
H36 H 0.3196 0.0483 0.5800 0.078 Uiso 1 1 calc R . .
C41 C 0.2241(15) 0.0244(11) 0.7207(11) 0.056(4) Uani 1 1 d . . .
C42 C 0.0905(15) -0.0251(11) 0.6548(10) 0.075(5) Uani 1 1 d . . .
H42 H 0.0124 0.0172 0.6504 0.090 Uiso 1 1 calc R . .
C43 C 0.0729(12) -0.1368(11) 0.5957(9) 0.074(5) Uani 1 1 d . . .
H43 H -0.0147 -0.1679 0.5498 0.088 Uiso 1 1 calc R . .
C44 C 0.1864(17) -0.2024(11) 0.6049(13) 0.089(6) Uani 1 1 d . . .
H44 H 0.1729 -0.2774 0.5706 0.107 Uiso 1 1 calc R . .
C45 C 0.3176(18) -0.1523(13) 0.6661(10) 0.077(5) Uani 1 1 d . . .
H45 H 0.3967 -0.1949 0.6667 0.093 Uiso 1 1 calc R . .
C46 C 0.3398(12) -0.0455(11) 0.7254(9) 0.065(5) Uani 1 1 d . . .
H46 H 0.4296 -0.0168 0.7695 0.078 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Mg1 N1 110.5(4) . . ?
C13 Mg1 N3 107.2(4) . . ?
N1 Mg1 N3 82.6(4) . . ?
C13 Mg1 C21 163.1(4) . . ?
N1 Mg1 C21 83.0(4) . . ?
N3 Mg1 C21 83.9(4) . . ?
C13 Mg1 C25 133.7(5) . . ?
N1 Mg1 C25 115.7(5) . . ?
N3 Mg1 C25 80.8(4) . . ?
C21 Mg1 C25 33.8(3) . . ?
C13 Mg1 C22 135.7(5) . . ?
N1 Mg1 C22 80.2(4) . . ?
N3 Mg1 C22 116.9(4) . . ?
C21 Mg1 C22 34.0(3) . . ?
C25 Mg1 C22 54.8(4) . . ?
C13 Mg1 C24 109.0(4) . . ?
N1 Mg1 C24 133.3(4) . . ?
N3 Mg1 C24 108.3(4) . . ?
C21 Mg1 C24 54.6(3) . . ?
C25 Mg1 C24 31.5(3) . . ?
C22 Mg1 C24 53.9(4) . . ?
C13 Mg1 C23 109.8(4) . . ?
N1 Mg1 C23 109.3(4) . . ?
N3 Mg1 C23 133.3(3) . . ?
C21 Mg1 C23 54.7(4) . . ?
C25 Mg1 C23 53.0(4) . . ?
C22 Mg1 C23 32.3(3) . . ?
C24 Mg1 C23 32.0(3) . . ?
C13 Si1 C14 107.4(5) . . ?
C13 Si1 C16 113.4(5) . . ?
C14 Si1 C16 109.8(5) . . ?
C13 Si1 C15 113.6(5) . . ?
C14 Si1 C15 106.8(4) . . ?
C16 Si1 C15 105.7(5) . . ?
C3 N1 N2 105.6(10) . . ?
C3 N1 Mg1 131.3(10) . . ?
N2 N1 Mg1 120.5(7) . . ?
C5 N2 N1 111.0(9) . . ?
C5 N2 C2 128.7(10) . . ?
N1 N2 C2 119.9(9) . . ?
C8 N3 N4 104.8(10) . . ?
C8 N3 Mg1 136.4(9) . . ?
N4 N3 Mg1 118.7(8) . . ?
C10 N4 N3 110.6(10) . . ?
C10 N4 C2 127.6(12) . . ?
N3 N4 C2 121.8(11) . . ?
C21 C1 C41 109.6(10) . . ?
C21 C1 C31 112.1(9) . . ?
C41 C1 C31 108.0(9) . . ?
C21 C1 C2 115.3(8) . . ?
C41 C1 C2 108.5(9) . . ?
C31 C1 C2 103.0(10) . . ?
N4 C2 N2 107.7(8) . . ?
N4 C2 C1 114.0(8) . . ?
N2 C2 C1 113.8(10) . . ?
N1 C3 C4 108.8(11) . . ?
N1 C3 C6 121.4(13) . . ?
C4 C3 C6 129.7(10) . . ?
C5 C4 C3 108.8(11) . . ?
C4 C5 N2 105.7(12) . . ?
C4 C5 C7 130.8(12) . . ?
N2 C5 C7 123.0(11) . . ?
N3 C8 C9 110.0(10) . . ?
N3 C8 C11 119.6(12) . . ?
C9 C8 C11 130.4(12) . . ?
C10 C9 C8 105.9(11) . . ?
N4 C10 C9 108.7(10) . . ?
N4 C10 C12 124.4(13) . . ?
C9 C10 C12 126.8(15) . . ?
Si1 C13 Mg1 123.6(5) . . ?
C25 C21 C22 105.2(10) . . ?
C25 C21 C1 128.8(12) . . ?
C22 C21 C1 125.9(13) . . ?
C25 C21 Mg1 73.9(5) . . ?
C22 C21 Mg1 74.6(5) . . ?
C1 C21 Mg1 114.0(5) . . ?
C23 C22 C21 107.5(12) . . ?
C23 C22 Mg1 76.3(6) . . ?
C21 C22 Mg1 71.3(5) . . ?
C24 C23 C22 108.7(13) . . ?
C24 C23 Mg1 73.5(6) . . ?
C22 C23 Mg1 71.4(6) . . ?
C25 C24 C23 108.4(13) . . ?
C25 C24 Mg1 71.3(6) . . ?
C23 C24 Mg1 74.5(6) . . ?
C24 C25 C21 110.2(12) . . ?
C24 C25 Mg1 77.2(6) . . ?
C21 C25 Mg1 72.2(5) . . ?
C32 C31 C36 117.3(12) . . ?
C32 C31 C1 123.0(9) . . ?
C36 C31 C1 119.7(14) . . ?
C33 C32 C31 120.1(11) . . ?
C32 C33 C34 122.2(13) . . ?
C35 C34 C33 118.6(11) . . ?
C36 C35 C34 120.1(11) . . ?
C35 C36 C31 121.7(14) . . ?
C42 C41 C46 116.9(11) . . ?
C42 C41 C1 125.0(10) . . ?
C46 C41 C1 118.1(12) . . ?
C43 C42 C41 120.9(11) . . ?
C42 C43 C44 120.5(12) . . ?
C45 C44 C43 117.5(12) . . ?
C46 C45 C44 124.3(12) . . ?
C45 C46 C41 119.7(12) . . ?
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
Mg1 C13 2.148(8) . ?
Mg1 N1 2.205(10) . ?
Mg1 N3 2.224(11) . ?
Mg1 C21 2.440(8) . ?
Mg1 C25 2.462(9) . ?
Mg1 C22 2.483(10) . ?
Mg1 C24 2.534(10) . ?
Mg1 C23 2.545(11) . ?
Si1 C13 1.840(10) . ?
Si1 C14 1.886(10) . ?
Si1 C16 1.889(13) . ?
Si1 C15 1.895(9) . ?
N1 C3 1.346(13) . ?
N1 N2 1.377(12) . ?
N2 C5 1.374(13) . ?
N2 C2 1.503(15) . ?
N3 C8 1.376(13) . ?
N3 N4 1.405(12) . ?
N4 C10 1.329(14) . ?
N4 C2 1.450(14) . ?
C1 C21 1.540(14) . ?
C1 C41 1.556(17) . ?
C1 C31 1.601(19) . ?
C1 C2 1.615(13) . ?
C3 C4 1.398(13) . ?
C3 C6 1.486(17) . ?
C4 C5 1.346(15) . ?
C5 C7 1.495(14) . ?
C8 C9 1.396(14) . ?
C8 C11 1.479(14) . ?
C9 C10 1.391(13) . ?
C10 C12 1.522(14) . ?
C21 C25 1.425(14) . ?
C21 C22 1.442(15) . ?
C22 C23 1.401(13) . ?
C23 C24 1.399(14) . ?
C24 C25 1.357(14) . ?
C31 C32 1.401(17) . ?
C31 C36 1.420(13) . ?
C32 C33 1.372(17) . ?
C33 C34 1.388(12) . ?
C34 C35 1.389(17) . ?
C35 C36 1.371(19) . ?
C41 C42 1.401(14) . ?
C41 C46 1.440(16) . ?
C42 C43 1.395(15) . ?
C43 C44 1.400(18) . ?
C44 C45 1.363(15) . ?
C45 C46 1.341(16) . ?
