Pyridyl donor induced 1,3-silyl migration in metal complexes of the guanidine CyHNC{N(SiMe3)Py}NCy, Py = 2-(6-MeC5H3N)
Cole, Marcus L.; Junk, Peter C.; Dalton Transactions  (2003) 2109–; doi:10.1039/b303772j

data_7013050
_publ_section_title
;
 Pyridyl donor induced 1,3-silyl migration in metal complexes of the
 guanidine CyHNC{N(SiMe3)Py}NCy, Py = 2-(6-MeC5H3N)
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2109
_journal_paper_doi               10.1039/b303772j
_journal_year                    2003
_chemical_formula_sum            'C30 H57 N4 Na O4 Si'
_chemical_formula_weight         588.88
_chemical_name_common            '[Na(DCCAMPTMS)(DME)2]'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.943(2)
_cell_length_b                   12.892(3)
_cell_length_c                   12.249(2)
_cell_measurement_temperature    123(2)
_cell_volume                     1727.2(6)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'X -Seed'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_sigmaI/netI    0.1641
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10293
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9769
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'performed as part of the DENZO-SMN package'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prisms'
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881
;
_refine_ls_abs_structure_Flack   -0.29(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6179
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                3585
_reflns_number_total             6179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303772j.txt
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7013050