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_4336536
_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         'C46 H54 Ca N4 O2 Si2'
_chemical_formula_sum            'C46 H54 Ca N4 O2 Si2'
_chemical_formula_weight         791.19
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 102.838(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0470(5)
_cell_length_b                   18.5192(6)
_cell_length_c                   16.9551(6)
_cell_measurement_reflns_used    12921
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.6318
_cell_measurement_theta_min      3.5810
_cell_volume                     4300.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18733
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         3.58
_diffrn_standards_decay_%        0
_diffrn_standards_number         20154
_exptl_absorpt_coefficient_mu    2.112
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.364
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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    1.222
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.14
_refine_diff_density_min         -1.55
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         7479
_refine_ls_number_restraints     2913
_refine_ls_restrained_S_all      0.97
_refine_ls_R_factor_all          0.144
_refine_ls_R_factor_gt           0.126
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+45.13P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.241
_refine_ls_wR_factor_ref         0.250
_reflns_number_gt                6338
_reflns_number_total             7479
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic4012923_si_001_2.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4336536
_nottingham_internal_coll_name   CEFOLA
_nottingham_internal_coll_number 9806
_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
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   12/3/2011
_nottingham_internal_process_user WL/AJB
_nottingham_internal_process_date 31/03/2011
_nottingham_internal_solution_user FO
_nottingham_internal_solution_date 23/07/2012
_nottingham_internal_refinement_user FO
_nottingham_internal_refinement_date 08/03/2013
_nottingham_internal_validation_user AJB
_nottingham_internal_archive_date 08/03/2013