N-Substituted Guanidinate Anions as Ancillary Ligands in Group 4 Chemistry. Syntheses and Characterization of M{RNC[N(SiMe3)2]NR}2Cl2, [M{CyNC[N(SiMe3)2]NCy}Cl3]- (M = Zr, Hf; R =iPr, Cy), and Zr{CyNC[N(SiMe3)2]NCy}(CH2Ph)3
Wood; Glenn P. A. Yap; Darrin S. Richeson; Inorganic Chemistry 38 (1999) 5788–5794; doi:10.1021/ic990668i

data_4322517
_publ_section_title
;
 N-Substituted Guanidinate Anions as Ancillary Ligands in Group 4
 Chemistry. Syntheses and Characterization of M{RNC[N(SiMe3)2]NR}2Cl2,
 [M{CyNC[N(SiMe3)2]NCy}Cl3]- (M = Zr, Hf; R =iPr, Cy), and
 Zr{CyNC[N(SiMe3)2]NCy}(CH2Ph)3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5788
_journal_page_last               5794
_journal_paper_doi               10.1021/ic990668i
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C40 H61 N3 Si2 Zr'
_chemical_formula_weight         731.32
_chemical_name_systematic
; 
 ? 
;
_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                 102.431(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.483(1)
_cell_length_b                   18.889(2)
_cell_length_c                   20.459(3)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     3956.2(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi 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  0.2136
_diffrn_reflns_av_sigmaI/netI    0.2548
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30927
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.928074
_exptl_absorpt_correction_T_min  0.501173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                2613
_reflns_number_total             4145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990668i_3.cif
_cod_data_source_block           dr153
_cod_original_cell_volume        3956.0(9)
_cod_database_code               4322517