Alkaline Earth Complexes of Silylated Aminopyridinato Ligands: Homoleptic Compounds and Heterobimetallic Coordination Polymers
Fabrizio Ortu; Graeme J. Moxey; Alexander J. Blake; William Lewis; Deborah L. Kays; Inorganic Chemistry 52 (2013) 12429–12439; doi:10.1021/ic4012923

data_4336535
_publ_contact_author_address
;  School of Chemistry, University of Nottingham,
   University Park,
   Nottingham, NG7 2RD, United Kingdom
;
_publ_contact_author_email       Deborah.Kays@nottingham.ac.uk
_publ_contact_author_fax         '+44-(0) 115 951 3461'
_publ_contact_author_name        'Deborah L. Kays'
_publ_contact_author_phone       '+49-(0) 115 951 3555'
_publ_section_title
;
 Alkaline Earth Complexes of Silylated Aminopyridinato Ligands: Homoleptic
 Compounds and Heterobimetallic Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12429
_journal_page_last               12439
_journal_paper_doi               10.1021/ic4012923
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C31 H53 Li Mg N6 O Si3'
_chemical_formula_sum            'C31 H53 Li Mg N6 O Si3'
_chemical_formula_weight         641.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-09-09
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.1281(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.05140(13)
_cell_length_b                   20.2091(3)
_cell_length_c                   18.6537(2)
_cell_measurement_reflns_used    13682
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      70.57
_cell_measurement_theta_min      4.49
_cell_volume                     3704.55(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.0750
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
  1 omega   23.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   30.0000 46

  2 omega  -26.00   14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   30.0000 40

  3 omega  -27.00   -2.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       -2.0000  125.0000   30.0000 25

  4 omega  -57.00  -31.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       -2.0000  125.0000  150.0000 26

  5 omega  -79.00  -54.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       -2.0000  178.0000  -90.0000 25

  6 omega   24.00   49.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000    3.6380 25

  7 omega   35.00   70.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  120.0000 35

  8 omega   23.00   49.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   55.9338 26

  9 omega  -18.00   26.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000 -150.0000 44

 10 omega   -8.00   18.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  120.0000 26

 11 omega   34.00   76.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000 -150.0000 42

 12 omega   23.00   48.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  116.3578 25

 13 omega   94.00  120.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 26

 14 omega   58.00  117.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000  -60.0000 59

 15 omega  100.00  143.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   90.0000 43

 16 omega  106.00  132.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   30.0000 26

 17 omega  115.00  173.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 58

 18 omega   45.00  100.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   60.0000 55

 19 omega   53.00   94.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 41

 20 omega   40.00   93.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 53

 21 omega   38.00  116.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 78

 22 omega   35.00   94.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 59

 23 omega   53.00  116.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 63

 24 omega   50.00  104.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -30.0000 54

 25 omega  -69.00   21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 90

 26 omega  -69.00   21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -30.0000 90

 27 omega   33.00  123.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 90

 28 omega   28.00   57.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000  -30.0000 29

 29 omega   23.00  111.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   90.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0336587000
_diffrn_orient_matrix_UB_12      0.0527539000
_diffrn_orient_matrix_UB_13      -0.0607475000
_diffrn_orient_matrix_UB_21      -0.0212790000
_diffrn_orient_matrix_UB_22      0.0516478000
_diffrn_orient_matrix_UB_23      0.0572772000
_diffrn_orient_matrix_UB_31      0.1516129000
_diffrn_orient_matrix_UB_32      0.0189766000
_diffrn_orient_matrix_UB_33      0.0128912000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_unetI/netI     0.020
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19407
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.724
_diffrn_reflns_theta_min         3.264
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  1.373
_exptl_absorpt_correction_T_min  1.020
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       rod
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.23
_refine_diff_density_rms         0.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.047P)^2^+1.407P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6353
_reflns_number_total             6866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4012923_si_001_1.cif
_cod_data_source_block           12
_cod_original_cell_volume        3704.53(9)
_cod_database_code               4336535
_nottingham_internal_coll_name   MGFOMK
_nottingham_internal_coll_number 12808
_nottingham_internal_coll_client FO/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '10 and 40s'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   FO
_nottingham_internal_coll_date   08/09/2013
_nottingham_internal_process_user FO
_nottingham_internal_process_date 09/09/2013
_nottingham_internal_solution_user FO
_nottingham_internal_solution_date 09/09/2013
_nottingham_internal_refinement_user FO
_nottingham_internal_refinement_date 09/09/2013
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 19/9/2013
_chemical_oxdiff_formula         'C31 H54 N6 Li Mg O Si3'
_chemical_oxdiff_usercomment
'MGFOMK #12808 FOR FO/DLK IN FOMBLIN FILM ON MICROMOUNT'
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. others
 Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=
 Sof(H30D)=Sof(H31C)=Sof(H31D)=1-FVAR(1)
 Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=
 Sof(H31A)=Sof(H31B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C28(H28C,H28D), C29(H29A,H29B), C29A(H29C,H29D), C30(H30A,
 H30B), C30A(H30C,H30D), C31(H31A,H31B), C31(H31C,H31D)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C20(H20), C21(H21),
 C22(H22)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              49344
_shelxl_version_number           2012-9