Synthesis and characterisation of novel zirconium(iv) derivatives containing the bis-amido ligand SiMe2(NRR')2
Passarelli, Vincenzo; Benetollo, Franco; Zanella, Pierino; Carta, Giovanni; Rossetto, Gilberto; Dalton Transactions  (2003) 1411–; doi:10.1039/b212705a

data_7012648
_publ_section_title
;
 Synthesis and characterisation of novel zirconium(iv) derivatives
 containing the bis-amido ligand SiMe2(NRR')2
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1411
_journal_paper_doi               10.1039/b212705a
_journal_year                    2003
_chemical_formula_moiety         Zr[(N^i^Pr)~2~SiMe~2~]~2~
_chemical_formula_sum            'C32 H80 N8 Si4 Zr2'
_chemical_formula_weight         871.84
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 110.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.033(3)
_cell_length_b                   46.986(5)
_cell_length_c                   10.498(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4647(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.879
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'Philips PW1100'
_diffrn_measurement_method       \Q/2\Q
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7761
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   '\Y scan'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+37.9809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.1796
_reflns_number_gt                6971
_reflns_number_total             7168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212705a.txt
_cod_data_source_block           zr-n2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7012648