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_4336537
_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         'C54 H90 Ca2 K2 N12 Si6'
_chemical_formula_sum            'C54 H90 Ca2 K2 N12 Si6'
_chemical_formula_weight         1234.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.877(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.265(4)
_cell_length_b                   11.2304(15)
_cell_length_c                   42.062(6)
_cell_measurement_reflns_used    10003
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      2.25
_cell_volume                     13937(3)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            49344
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  0.9707
_exptl_absorpt_correction_T_min  0.9308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       plate
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         12297
_refine_ls_number_restraints     420
_refine_ls_restrained_S_all      1.367
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.1104
_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^)+(0.0321P)^2^+128.8775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.1958
_reflns_number_gt                9463
_reflns_number_total             12297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012923_si_001_3.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4336537
_nottingham_internal_coll_name   CAFOLB
_nottingham_internal_coll_number 9617
_nottingham_internal_coll_client FO/DLK
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_time '40 s'
_nottingham_internal_coll_frame_width '0.3 degrees'
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   FO/WL
_nottingham_internal_coll_date   30/7/10
_nottingham_internal_process_user FO/WL
_nottingham_internal_process_date 02/08/2010
_nottingham_internal_solution_user FO
_nottingham_internal_solution_date 15/01/2013
_nottingham_internal_refinement_user FO
_nottingham_internal_refinement_date 15/01/2013
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 11/2/2013