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_4336538
_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         'C22 H39 Li Mg N4 Si2'
_chemical_formula_sum            'C22 H39 Li Mg N4 Si2'
_chemical_formula_weight         447.00
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 118.782(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4769(10)
_cell_length_b                   12.6948(5)
_cell_length_c                   13.5233(8)
_cell_measurement_reflns_used    5576
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.2269
_cell_measurement_theta_min      3.7262
_cell_volume                     2629.7(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10380
_diffrn_reflns_point_group_measured_fraction_full 0.878
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         4.524
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.1964
_exptl_crystal_size_mid          0.1387
_exptl_crystal_size_min          0.0976
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 1418 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.20(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     350
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0822P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    0.778
_reflns_Friedel_fraction_max     0.795
_reflns_number_gt                3597
_reflns_number_total             4168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4012923_si_001_4.cif
_cod_data_source_block           11
_cod_database_code               4336538
_nottingham_internal_coll_name   MGFOLC
_nottingham_internal_coll_number 9883
_nottingham_internal_coll_client FO/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '15 and 60s'
_nottingham_internal_coll_frame_width '1 degree'
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   wl
_nottingham_internal_coll_date   30/11/2010
_nottingham_internal_process_user wl
_nottingham_internal_process_date 03/12/2010
_nottingham_internal_solution_user FO
_nottingham_internal_solution_date 03/7/2013
_nottingham_internal_refinement_user FO
_nottingham_internal_refinement_date 03/7/2013
_shelxl_version_number           2012-9
_shelx_res_checksum              54415