Preparation of Zirconium Guanidinate Complexes from the Direct Insertion of a Carbodiimine and Aminolysis Using a Guanidine. Comparison of the Reactions
Chen, Shu-Jian; Dougan, Brenda A.; Chen, Xue-Tai; Xue, Zi-Ling; Organometallics 31 (2012) 3443–; doi:10.1021/om300097a

data_4078086
_publ_section_title
;
 Preparation of Zirconium Guanidinate Complexes from the Direct Insertion
 of a Carbodiimine and Aminolysis Using a Guanidine. Comparison of the
 Reactions
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3443
_journal_paper_doi               10.1021/om300097a
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C28 H67 N5 Si4 Zr'
_chemical_formula_sum            'C28 H67 N5 Si4 Zr'
_chemical_formula_weight         677.45
_chemical_name_common            'Guanidinate TriTMSsilyl Zr'
_chemical_name_systematic
; 
 Guanidinate TriTMSsilyl Zr 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                96.198(15)
_cell_angle_beta                 95.664(17)
_cell_angle_gamma                93.531(16)
_cell_formula_units_Z            2
_cell_length_a                   9.635(7)
_cell_length_b                   11.677(9)
_cell_length_c                   17.915(13)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.15
_cell_volume                     1989(3)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17014
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  0.9208
_exptl_absorpt_correction_T_min  0.8501
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0586P)^2^+0.4905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                6515
_reflns_number_total             6948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300097a_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078086