#------------------------------------------------------------------------------
#$Date: 2017-03-04 16:27:26 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193614 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/70/4087014.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_4087014
loop_
_publ_author_name
'Garcés, Andrés'
'Sánchez-Barba, Luis F.'
'Fernández-Baeza, Juan'
'Otero, Antonio'
'Lara-Sánchez, Agustín'
'Rodríguez, Ana M.'
_publ_section_title
;
 Studies on Multinuclear Magnesium tert-Butyl Heteroscorpionates:
 Synthesis, Coordination Ability, and Heteroselective Ring-Opening
 Polymerization of rac-Lactide
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              884
_journal_paper_doi               10.1021/acs.organomet.6b00934
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C42 H62 Mg2 N6 O2'
_chemical_formula_sum            'C42 H62 Mg2 N6 O2'
_chemical_formula_weight         731.59
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.350(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.935(4)
_cell_length_b                   17.911(6)
_cell_length_c                   18.857(5)
_cell_measurement_reflns_used    534
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      15.297
_cell_measurement_theta_min      2.274
_cell_volume                     4413(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'WINGX v2014.1 (Farrugia, 2012)'
_computing_publication_material  'WINGX v2014.1 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.767
_diffrn_measurement_device_type  'CCD X8 APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1063
_diffrn_reflns_av_unetI/netI     0.1739
_diffrn_reflns_Laue_measured_fraction_full 0.862
_diffrn_reflns_Laue_measured_fraction_max 0.767
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9327
_diffrn_reflns_point_group_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.767
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.436
_diffrn_reflns_theta_min         2.510
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4699
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.2581
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1205P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.2784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1328
_reflns_number_total             4699
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00934_si_002.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 4087009--4087016.cif.'
_cod_database_code               4087014
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg1 Mg 0.28384(12) 0.75411(9) 0.23812(11) 0.0773(6) Uani 1 1 d . U . . .
N5 N 0.4081(3) 0.71124(18) 0.2219(2) 0.0636(11) Uani 1 1 d . U . . .
N1 N 0.3317(11) 0.8670(9) 0.2106(11) 0.071(3) Uani 0.5 1 d D U P A 1
N2 N 0.4267(12) 0.8678(11) 0.2028(13) 0.068(4) Uani 0.5 1 d D U P A 1
C1 C 0.4348(11) 0.9263(9) 0.1590(11) 0.071(4) Uani 0.5 1 d D U P A 1
C2 C 0.3402(11) 0.9587(9) 0.1328(11) 0.084(5) Uani 0.5 1 d D U P A 1
H2 H 0.3206 0.9983 0.0989 0.100 Uiso 0.5 1 calc R U P A 1
C3 C 0.2792(11) 0.9226(9) 0.1653(11) 0.078(5) Uani 0.5 1 d D U P A 1
C4 C 0.5325(11) 0.9416(12) 0.1437(13) 0.093(5) Uani 0.5 1 d D U P A 1
H4A H 0.5165 0.9657 0.0954 0.139 Uiso 0.5 1 calc R U P A 1
H4B H 0.5672 0.8954 0.1433 0.139 Uiso 0.5 1 calc R U P A 1
H4C H 0.5760 0.9735 0.1825 0.139 Uiso 0.5 1 calc R U P A 1
C5 C 0.1695(10) 0.9351(10) 0.1552(13) 0.102(6) Uani 0.5 1 d D U P A 1
H5A H 0.1457 0.9796 0.1260 0.153 Uiso 0.5 1 calc R U P A 1
H5B H 0.1625 0.9406 0.2038 0.153 Uiso 0.5 1 calc R U P A 1
H5C H 0.1296 0.8932 0.1293 0.153 Uiso 0.5 1 calc R U P A 1
N1A N 0.3095(12) 0.8561(10) 0.2156(13) 0.089(4) Uani 0.5 1 d D U P A 2
N2A N 0.4032(12) 0.8694(10) 0.2078(13) 0.072(4) Uani 0.5 1 d D U P A 2
C1A C 0.3981(13) 0.9277(11) 0.1594(14) 0.095(6) Uani 0.5 1 d D U P A 2
C2A C 0.2999(12) 0.9529(10) 0.1382(12) 0.096(6) Uani 0.5 1 d D U P A 2
H2A H 0.2731 0.9933 0.1064 0.115 Uiso 0.5 1 calc R U P A 2
C3A C 0.2468(12) 0.9085(10) 0.1716(13) 0.095(5) Uani 0.5 1 d D U P A 2
C4A C 0.4894(12) 0.9509(11) 0.1406(13) 0.095(6) Uani 0.5 1 d D U P A 2
H4A1 H 0.4678 0.9820 0.0963 0.142 Uiso 0.5 1 calc R U P A 2
H4A2 H 0.5233 0.9074 0.1311 0.142 Uiso 0.5 1 calc R U P A 2
H4A3 H 0.5357 0.9783 0.1822 0.142 Uiso 0.5 1 calc R U P A 2
C5A C 0.1360(10) 0.9092(10) 0.1622(13) 0.109(6) Uani 0.5 1 d D U P A 2
H5A1 H 0.0971 0.9290 0.1134 0.163 Uiso 0.5 1 calc R U P A 2
H5A2 H 0.1260 0.9397 0.2009 0.163 Uiso 0.5 1 calc R U P A 2
H5A3 H 0.1138 0.8591 0.1664 0.163 Uiso 0.5 1 calc R U P A 2
C11 C 0.5000 0.8250(3) 0.2500 0.0666(18) Uani 1 2 d S TU P . .
C12 C 0.5000 0.7473(3) 0.2500 0.0616(17) Uani 1 2 d S TU P A .
C13 C 0.4041(3) 0.6439(2) 0.1833(3) 0.0604(12) Uani 1 1 d . U . . .
C14 C 0.4525(3) 0.6336(3) 0.1314(3) 0.0688(13) Uani 1 1 d . U . . .
H14 H 0.4959 0.6707 0.1256 0.083 Uiso 1 1 calc R U . . .
C15 C 0.4387(4) 0.5702(3) 0.0882(3) 0.0767(15) Uani 1 1 d . U . . .
H15 H 0.4733 0.5652 0.0543 0.092 Uiso 1 1 calc R U . . .
C16 C 0.3747(4) 0.5137(2) 0.0940(3) 0.0712(14) Uani 1 1 d . U . . .
C17 C 0.3268(4) 0.5243(3) 0.1456(3) 0.0809(15) Uani 1 1 d . U . . .
H17 H 0.2825 0.4874 0.1504 0.097 Uiso 1 1 calc R U . . .
C18 C 0.3411(3) 0.5868(2) 0.1908(3) 0.0715(14) Uani 1 1 d . U . . .
H18 H 0.3085 0.5906 0.2261 0.086 Uiso 1 1 calc R U . . .
C19 C 0.3576(5) 0.4445(3) 0.0442(4) 0.107(2) Uani 1 1 d . U . . .
H19A H 0.3697 0.4565 -0.0016 0.161 Uiso 1 1 calc R U . . .
H19B H 0.2883 0.4276 0.0321 0.161 Uiso 1 1 calc R U . . .
H19C H 0.4038 0.4058 0.0707 0.161 Uiso 1 1 calc R U . . .
C20 C 0.2343(5) 0.7371(4) 0.3312(4) 0.1013(18) Uani 1 1 d D U . . .
C21 C 0.3229(13) 0.7408(11) 0.4050(11) 0.177(8) Uani 0.5 1 d D U P B 1
H21A H 0.3662 0.7821 0.4039 0.265 Uiso 0.5 1 calc R U P B 1
H21B H 0.3614 0.6952 0.4124 0.265 Uiso 0.5 1 calc R U P B 1
H21C H 0.2974 0.7474 0.4458 0.265 Uiso 0.5 1 calc R U P B 1
C22 C 0.1532(13) 0.7937(10) 0.3323(18) 0.112(6) Uani 0.5 1 d D U P B 1
H22A H 0.1316 0.7835 0.3744 0.167 Uiso 0.5 1 calc R U P B 1
H22B H 0.0955 0.7900 0.2861 0.167 Uiso 0.5 1 calc R U P B 1
H22C H 0.1814 0.8431 0.3370 0.167 Uiso 0.5 1 calc R U P B 1
C23 C 0.1805(12) 0.6586(7) 0.3340(11) 0.124(6) Uani 0.5 1 d D U P B 1
H23A H 0.1668 0.6549 0.3804 0.186 Uiso 0.5 1 calc R U P B 1
H23B H 0.2251 0.6186 0.3314 0.186 Uiso 0.5 1 calc R U P B 1
H23C H 0.1174 0.6551 0.2919 0.186 Uiso 0.5 1 calc R U P B 1
C21A C 0.3144(10) 0.7864(8) 0.3977(9) 0.099(4) Uani 0.5 1 d D U P B 2
H21D H 0.2964 0.7838 0.4424 0.148 Uiso 0.5 1 calc R U P B 2
H21E H 0.3120 0.8373 0.3815 0.148 Uiso 0.5 1 calc R U P B 2
H21F H 0.3824 0.7671 0.4086 0.148 Uiso 0.5 1 calc R U P B 2
C22A C 0.1323(14) 0.7731(11) 0.3205(19) 0.111(6) Uani 0.5 1 d D U P B 2
H22D H 0.0786 0.7442 0.2854 0.166 Uiso 0.5 1 calc R U P B 2
H22E H 0.1314 0.8227 0.3011 0.166 Uiso 0.5 1 calc R U P B 2
H22F H 0.1220 0.7753 0.3682 0.166 Uiso 0.5 1 calc R U P B 2
C23A C 0.2464(12) 0.6618(8) 0.3583(11) 0.115(5) Uani 0.5 1 d D U P B 2
H23D H 0.2430 0.6605 0.4083 0.172 Uiso 0.5 1 calc R U P B 2
H23E H 0.3115 0.6429 0.3597 0.172 Uiso 0.5 1 calc R U P B 2
H23F H 0.1927 0.6314 0.3251 0.172 Uiso 0.5 1 calc R U P B 2
O1 O 0.1717(3) 0.7313(2) 0.1373(2) 0.0937(12) Uani 1 1 d D U . . .
C27 C 0.1860(4) 0.7410(3) 0.0650(4) 0.0980(17) Uani 1 1 d D U . . .
H27A H 0.2528 0.7231 0.0674 0.118 Uiso 1 1 calc R U . C 1
H27B H 0.1794 0.7931 0.0499 0.118 Uiso 1 1 calc R U . C 1
C24 C 0.0931(12) 0.6741(9) 0.1359(8) 0.107(4) Uani 0.5 1 d D U P D 1
H24A H 0.0467 0.6926 0.1602 0.128 Uiso 0.5 1 calc R U P D 1
H24B H 0.1248 0.6283 0.1607 0.128 Uiso 0.5 1 calc R U P D 1
C25 C 0.0375(11) 0.6619(11) 0.0513(10) 0.128(5) Uani 0.5 1 d D U P D 1
H25A H 0.0279 0.6090 0.0402 0.153 Uiso 0.5 1 calc R U P D 1
H25B H -0.0290 0.6858 0.0351 0.153 Uiso 0.5 1 calc R U P D 1
C26 C 0.1028(12) 0.6953(12) 0.0118(10) 0.124(5) Uani 0.5 1 d D U P D 1
H26A H 0.0610 0.7265 -0.0295 0.149 Uiso 0.5 1 calc R U P D 1
H26B H 0.1323 0.6559 -0.0094 0.149 Uiso 0.5 1 calc R U P D 1
C24A C 0.0726(14) 0.7002(10) 0.1143(9) 0.117(5) Uani 0.5 1 d D U P D 2
H24C H 0.0205 0.7373 0.0909 0.141 Uiso 0.5 1 calc R U P D 2
H24D H 0.0588 0.6772 0.1563 0.141 Uiso 0.5 1 calc R U P D 2
C25A C 0.0798(11) 0.6415(10) 0.0564(10) 0.117(4) Uani 0.5 1 d D U P D 2
H25C H 0.1131 0.5964 0.0817 0.141 Uiso 0.5 1 calc R U P D 2
H25D H 0.0123 0.6287 0.0213 0.141 Uiso 0.5 1 calc R U P D 2
C26A C 0.1422(13) 0.6788(12) 0.0165(11) 0.114(5) Uani 0.5 1 d D U P D 2
H26C H 0.1950 0.6458 0.0121 0.137 Uiso 0.5 1 calc R U P D 2
H26D H 0.0997 0.6955 -0.0335 0.137 Uiso 0.5 1 calc R U P D 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 0.0000 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'
O O 0.0106 0.0060 '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
N1A Mg1 N5 95.3(5) . .
N1A Mg1 O1 97.1(7) . .
N5 Mg1 O1 101.71(17) . .
N1A Mg1 C20 117.1(7) . .
N5 Mg1 C20 128.0(2) . .
O1 Mg1 C20 112.3(2) . .
N5 Mg1 N1 88.2(4) . .
O1 Mg1 N1 99.0(5) . .
C20 Mg1 N1 122.0(6) . .
C12 N5 C13 118.2(4) . .
C12 N5 Mg1 120.1(3) . .
C13 N5 Mg1 121.8(3) . .
C3 N1 N2 104.8(10) . .
C3 N1 Mg1 132.1(12) . .
N2 N1 Mg1 114.0(10) . .
C11 N2 C1 129.7(12) . .
C11 N2 N1 117.5(11) . .
C1 N2 N1 110.9(10) . .
N2 C1 C2 105.8(11) . .
N2 C1 C4 121.7(11) . .
C2 C1 C4 132.4(11) . .
C1 C2 C3 108.0(10) . .
N1 C3 C2 110.3(10) . .
N1 C3 C5 119.9(12) . .
C2 C3 C5 129.7(11) . .
C3A N1A N2A 104.4(11) . .
C3A N1A Mg1 131.3(13) . .
N2A N1A Mg1 116.0(11) . .
C1A N2A N1A 111.6(11) . .
C1A N2A C11 125.0(12) . .
N1A N2A C11 123.3(11) . .
N2A C1A C2A 105.2(11) . .
N2A C1A C4A 121.2(13) . .
C2A C1A C4A 133.6(13) . .
C1A C2A C3A 108.6(11) . .
N1A C3A C2A 110.2(12) . .
N1A C3A C5A 120.0(12) . .
C2A C3A C5A 129.7(12) . .
N2 C11 N2 110(2) 2_655 .
N2 C11 C12 125.0(11) 2_655 .
N2 C11 C12 125.0(11) . .
C12 C11 N2A 121.3(8) . .
C12 C11 N2A 121.3(8) . 2_655
N2A C11 N2A 117.4(16) . 2_655
N5 C12 N5 123.6(5) 2_655 .
N5 C12 C11 118.2(3) 2_655 .
N5 C12 C11 118.2(3) . .
C14 C13 C18 117.1(4) . .
C14 C13 N5 122.9(4) . .
C18 C13 N5 119.7(4) . .
C15 C14 C13 122.0(4) . .
C14 C15 C16 121.5(5) . .
C17 C16 C15 116.3(5) . .
C17 C16 C19 122.6(5) . .
C15 C16 C19 121.1(5) . .
C16 C17 C18 123.4(5) . .
C17 C18 C13 119.8(5) . .
C23A C20 C22A 116.0(13) . .
C21 C20 C22 109.3(11) . .
C21 C20 C23 104.5(9) . .
C22 C20 C23 103.0(10) . .
C23A C20 C21A 105.8(10) . .
C22A C20 C21A 103.5(11) . .
C23A C20 Mg1 113.6(8) . .
C22A C20 Mg1 113.0(14) . .
C21 C20 Mg1 111.1(10) . .
C22 C20 Mg1 111.9(13) . .
C23 C20 Mg1 116.4(8) . .
C21A C20 Mg1 103.1(7) . .
C24A O1 C27 101.4(7) . .
C27 O1 C24 113.9(6) . .
C24A O1 Mg1 135.8(7) . .
C27 O1 Mg1 122.6(3) . .
C24 O1 Mg1 118.2(6) . .
C26A C27 O1 109.7(9) . .
O1 C27 C26 103.7(7) . .
O1 C24 C25 102.6(10) . .
C26 C25 C24 106.9(10) . .
C25 C26 C27 110.6(11) . .
O1 C24A C25A 100.9(12) . .
C26A C25A C24A 104.0(12) . .
C27 C26A C25A 102.7(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 N1A 1.937(15) .
Mg1 N5 2.013(4) .
Mg1 O1 2.039(4) .
Mg1 C20 2.119(7) .
Mg1 N1 2.246(14) .
N5 C12 1.365(4) .
N5 C13 1.400(5) .
N1 C3 1.349(12) .
N1 N2 1.381(11) .
N2 C11 1.338(15) .
N2 C1 1.364(12) .
C1 C2 1.367(13) .
C1 C4 1.511(13) .
C2 C3 1.371(14) .
C3 C5 1.490(13) .
N1A C3A 1.352(12) .
N1A N2A 1.383(11) .
N2A C1A 1.373(12) .
N2A C11 1.529(14) .
C1A C2A 1.362(14) .
C1A C4A 1.494(13) .
C2A C3A 1.378(14) .
C3A C5A 1.492(13) .
C11 N2 1.338(15) 2_655
C11 C12 1.392(8) .
C11 N2A 1.529(14) 2_655
C12 N5 1.365(4) 2_655
C13 C14 1.381(6) .
C13 C18 1.387(6) .
C14 C15 1.371(6) .
C15 C16 1.377(6) .
C16 C17 1.371(6) .
C16 C19 1.523(7) .
C17 C18 1.378(6) .
C20 C23A 1.431(15) .
C20 C22A 1.509(18) .
C20 C21 1.507(16) .
C20 C22 1.523(15) .
C20 C23 1.603(13) .
C20 C21A 1.620(15) .
O1 C24A 1.410(16) .
O1 C27 1.455(7) .
O1 C24 1.494(12) .
C27 C26A 1.435(18) .
C27 C26 1.488(14) .
C24 C25 1.528(17) .
C25 C26 1.488(13) .
C24A C25A 1.543(17) .
C25A C26A 1.493(13) .
