Synthesis and structures of selected benzamidinates of Li, Na, Al, Zr and Sn(II) using the C1-symmetric ligands [N(SiMe3)C(C6H4Me-4 or Ph)NPh]-.
Hitchcock, Peter B.; Lappert, Michael F.; Merle, Philippe G.; Dalton transactions (Cambridge, England : 2003)  (2007) 585–594; doi:10.1039/b614351b

data_7004983
_publ_section_title
;
 Synthesis and structures of selected benzamidinates of Li, Na, Al, Zr
 and Sn(II) using the C1-symmetric ligands [N(SiMe3)C(C6H4Me-4 or
 Ph)NPh]-.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              585
_journal_page_last               594
_journal_paper_doi               10.1039/b614351b
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C51 H63 Cl1 N6 Si3 Zr1, 3(C7 H8)'
_chemical_formula_sum            'C72 H87 Cl N6 Si3 Zr'
_chemical_formula_weight         1247.42
_chemical_name_common            '[ZrCl{Me3SiNC(C6H4Me)NPh}3].3(toluene)'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-12-07T10:21:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                114.887(2)
_cell_angle_beta                 98.208(2)
_cell_angle_gamma                105.088(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1992(5)
_cell_length_b                   16.9004(7)
_cell_length_c                   17.7967(7)
_cell_measurement_reflns_used    68640
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      4.246
_cell_measurement_wavelength     0.71073
_cell_volume                     3582.0(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32825
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         4.27
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         12331
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0818
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+14.9844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2258
_reflns_number_gt                9899
_reflns_number_total             12331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b614351b.txt
_cod_data_source_block           (6)-dec599
_cod_original_cell_volume        3582.0(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004983