Transition Metal Complexes of Guanidinate Dianions: Reactions between Guanidines and M(NMe2)5 (M = Ta, Nb)
Ma K. T. Tin; Glenn P. A. Yap; Darrin S. Richeson; Inorganic Chemistry 37 (1998) 6728–6730; doi:10.1021/ic980736l

data_4323255
_publ_section_title
;
 Transition Metal Complexes of Guanidinate Dianions: Reactions between
 Guanidines and M(NMe2)5 (M = Ta, Nb)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6728
_journal_page_last               6730
_journal_paper_doi               10.1021/ic980736l
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C25 H51 N6 Ta'
_chemical_formula_weight         616.67
_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                117.075(1)
_cell_angle_beta                 101.744(1)
_cell_angle_gamma                98.507(1)
_cell_formula_units_Z            2
_cell_length_a                   9.4155(2)
_cell_length_b                   13.3188(2)
_cell_length_c                   13.5215(2)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      23.50
_cell_measurement_theta_min      1.78
_cell_volume                     1420.81(5)
_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_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  0.089
_diffrn_reflns_av_sigmaI/netI    0.106
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9879
_diffrn_reflns_theta_full        20.91
_diffrn_reflns_theta_max         20.91
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    3.890
_exptl_absorpt_correction_T_max  0.694497
_exptl_absorpt_correction_T_min  0.322575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.264
_refine_diff_density_min         -4.201
_refine_diff_density_rms         1.023
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.005
_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          0.1039
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                4193
_reflns_number_total             4187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980736l.cif
_cod_data_source_block           dr015
_cod_original_cell_volume        1420.81(4)
_cod_database_code               4323255