#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/32/4323255.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4323255
loop_
_publ_author_name
'Ma K. T. Tin'
'Glenn P. A. Yap'
'Darrin S. Richeson'
_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
_chemical_name_systematic
; 
 ? 
;
_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/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta Ta 0.7165(1) 0.3530(1) 0.0853(1) 0.024(1) Uani 1 1 d . . .
N1 N 0.5024(13) 0.3044(10) 0.0852(10) 0.026(3) Uani 1 1 d . . .
N2 N 0.2996(13) 0.1613(10) -0.0828(10) 0.029(3) Uani 1 1 d . . .
N3 N 0.5483(12) 0.2618(9) -0.0799(10) 0.024(3) Uani 1 1 d . . .
N4 N 0.8304(14) 0.2356(10) 0.0512(10) 0.031(3) Uani 1 1 d . . .
N5 N 0.8014(13) 0.4931(10) 0.0776(10) 0.028(3) Uani 1 1 d . . .
N6 N 0.8150(13) 0.4324(9) 0.2548(11) 0.032(3) Uani 1 1 d . . .
C1 C 0.4424(19) 0.4084(13) 0.2683(12) 0.033(4) Uani 1 1 d . . .
H1A H 0.4134 0.4644 0.2456 0.040 Uiso 1 1 calc R . .
H1B H 0.5499 0.4396 0.3130 0.040 Uiso 1 1 calc R . .
C2 C 0.3516(17) 0.3956(13) 0.3444(13) 0.033(4) Uani 1 1 d . . .
H2A H 0.2438 0.3725 0.3025 0.040 Uiso 1 1 calc R . .
H2B H 0.3747 0.4715 0.4155 0.040 Uiso 1 1 calc R . .
C3 C 0.3853(21) 0.3046(14) 0.3778(14) 0.044(4) Uani 1 1 d . . .
H3A H 0.4897 0.3325 0.4285 0.053 Uiso 1 1 calc R . .
H3B H 0.3186 0.2945 0.4214 0.053 Uiso 1 1 calc R . .
C4 C 0.3625(21) 0.1868(14) 0.2695(15) 0.048(5) Uani 1 1 d . . .
H4A H 0.3939 0.1321 0.2934 0.057 Uiso 1 1 calc R . .
H4B H 0.2553 0.1535 0.2242 0.057 Uiso 1 1 calc R . .
C5 C 0.4534(18) 0.2013(13) 0.1940(14) 0.035(4) Uani 1 1 d . . .
H5A H 0.4323 0.1255 0.1231 0.042 Uiso 1 1 calc R . .
H5B H 0.5612 0.2259 0.2365 0.042 Uiso 1 1 calc R . .
C6 C 0.4169(16) 0.2919(12) 0.1598(11) 0.022(3) Uani 1 1 d . . .
H6A H 0.3084 0.2639 0.1149 0.027 Uiso 1 1 calc R . .
C7 C 0.0531(15) 0.0653(12) -0.2253(13) 0.032(4) Uani 1 1 d . . .
H7A H 0.0322 0.1418 -0.1984 0.038 Uiso 1 1 calc R . .
H7B H 0.0224 0.0331 -0.1782 0.038 Uiso 1 1 calc R . .
C8 C -0.0403(18) -0.0176(14) -0.3547(13) 0.041(4) Uani 1 1 d . . .
H8A H -0.0185 0.0185 -0.4009 0.049 Uiso 1 1 calc R . .
H8B H -0.1481 -0.0305 -0.3625 0.049 Uiso 1 1 calc R . .
C9 C -0.0009(19) -0.1377(14) -0.4017(15) 0.048(5) Uani 1 1 d . . .
H9A H -0.0351 -0.1783 -0.3623 0.058 Uiso 1 1 calc R . .
H9B H -0.0542 -0.1871 -0.4855 0.058 Uiso 1 1 calc R . .
C10 C 0.1667(18) -0.1201(13) -0.3813(14) 0.042(4) Uani 1 1 d . . .
H10A H 0.1984 -0.0883 -0.4284 0.051 Uiso 1 1 calc R . .
H10B H 0.1887 -0.1961 -0.4068 0.051 Uiso 1 1 calc R . .
C11 C 0.2570(18) -0.0365(12) -0.2524(13) 0.032(4) Uani 1 1 d . . .
H11A H 0.2322 -0.0716 -0.2061 0.039 Uiso 1 1 calc R . .
H11B H 0.3651 -0.0252 -0.2434 0.039 Uiso 1 1 calc R . .
C12 C 0.2231(15) 0.0817(12) -0.2070(12) 0.025(3) Uani 1 1 d . . .
H12A H 0.2546 0.1189 -0.2509 0.029 Uiso 1 1 calc R . .
C13 C 0.4501(16) 0.2727(13) -0.2604(12) 0.027(4) Uani 1 1 d . . .
H13A H 0.3494 0.2665 -0.2506 0.032 Uiso 1 1 calc R . .
H13B H 0.5039 0.3562 -0.2208 0.032 Uiso 1 1 calc R . .
C14 C 0.4350(19) 0.2184(16) -0.3866(14) 0.046(5) Uani 1 1 d . . .
H14A H 0.3800 0.2589 -0.4193 0.055 Uiso 1 1 calc R . .
H14B H 0.3755 0.1363 -0.4268 0.055 Uiso 1 1 calc R . .
C15 C 0.5889(21) 0.2239(19) -0.4097(15) 0.055(5) Uani 1 1 d . . .
H15A H 0.5740 0.1814 -0.4938 0.066 Uiso 1 1 calc R . .
H15B H 0.6449 0.3057 -0.3780 0.066 Uiso 1 1 calc R . .
C16 C 0.6778(19) 0.1678(16) -0.3503(14) 0.043(4) Uani 1 1 d . . .
H16A H 0.6276 0.0837 -0.3901 0.052 Uiso 1 1 calc R . .
H16B H 0.7793 0.1769 -0.3584 0.052 Uiso 1 1 calc R . .
C17 C 0.6911(16) 0.2220(14) -0.2211(13) 0.032(4) Uani 1 1 d . . .
H17A H 0.7494 0.3046 -0.1795 0.039 Uiso 1 1 calc R . .
H17B H 0.7452 0.1813 -0.1882 0.039 Uiso 1 1 calc R . .
C18 C 0.5357(15) 0.2134(13) -0.2036(12) 0.026(3) Uani 1 1 d . . .
H18A H 0.4798 0.1293 -0.2451 0.031 Uiso 1 1 calc R . .
C19 C 0.4317(16) 0.2325(12) -0.0394(13) 0.025(3) Uani 1 1 d . . .
C20 C 0.7552(20) 0.1084(13) -0.0158(15) 0.046(4) Uani 1 1 d . . .
H20A H 0.6466 0.0956 -0.0358 0.069 Uiso 1 1 calc R . .
H20B H 0.7861 0.0733 0.0312 0.069 Uiso 1 1 calc R . .
H20C H 0.7834 0.0727 -0.0866 0.069 Uiso 1 1 calc R . .
C21 C 0.9934(16) 0.2602(15) 0.0836(15) 0.046(5) Uani 1 1 d . . .
H21A H 1.0385 0.3444 0.1273 0.068 Uiso 1 1 calc R . .
H21B H 1.0240 0.2261 0.0137 0.068 Uiso 1 1 calc R . .
H21C H 1.0268 0.2266 0.1315 0.068 Uiso 1 1 calc R . .
C22 C 0.7161(18) 0.5413(13) 0.0115(14) 0.038(4) Uani 1 1 d . . .
H22A H 0.6132 0.4917 -0.0290 0.057 Uiso 1 1 calc R . .
H22B H 0.7643 0.5433 -0.0448 0.057 Uiso 1 1 calc R . .
H22C H 0.7156 0.6202 0.0655 0.057 Uiso 1 1 calc R . .
C23 C 0.9541(17) 0.5675(15) 0.1373(16) 0.046(5) Uani 1 1 d . . .
H23A H 1.0103 0.5369 0.1805 0.070 Uiso 1 1 calc R . .
H23B H 0.9530 0.6463 0.1909 0.070 Uiso 1 1 calc R . .
H23C H 1.0017 0.5693 0.0807 0.070 Uiso 1 1 calc R . .
C24 C 0.8368(20) 0.5577(13) 0.3420(13) 0.042(4) Uani 1 1 d . . .
H24A H 0.7995 0.5978 0.3020 0.064 Uiso 1 1 calc R . .
H24B H 0.9433 0.5952 0.3843 0.064 Uiso 1 1 calc R . .
H24C H 0.7817 0.5618 0.3964 0.064 Uiso 1 1 calc R . .
C25 C 0.8748(20) 0.3774(15) 0.3232(14) 0.043(4) Uani 1 1 d . . .
H25A H 0.8633 0.2953 0.2703 0.065 Uiso 1 1 calc R . .
H25B H 0.8191 0.3839 0.3778 0.065 Uiso 1 1 calc R . .
H25C H 0.9808 0.4173 0.3657 0.065 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ta N6 93.4(5) . . ?
N4 Ta N5 116.1(5) . . ?
N6 Ta N5 92.3(5) . . ?
N4 Ta N1 117.6(5) . . ?
N6 Ta N1 97.7(4) . . ?
N5 Ta N1 124.4(5) . . ?
N4 Ta N3 96.2(4) . . ?
N6 Ta N3 161.6(4) . . ?
N5 Ta N3 97.5(4) . . ?
N1 Ta N3 63.8(4) . . ?
N4 Ta C19 105.3(4) . . ?
N6 Ta C19 130.0(4) . . ?
N5 Ta C19 118.0(4) . . ?
N1 Ta C19 32.6(4) . . ?
N3 Ta C19 31.8(4) . . ?
C19 N1 C6 117.1(11) . . ?
C19 N1 Ta 98.4(8) . . ?
C6 N1 Ta 141.5(9) . . ?
C19 N2 C12 125.1(12) . . ?
C19 N3 C18 123.8(12) . . ?
C19 N3 Ta 95.5(8) . . ?
C18 N3 Ta 139.6(8) . . ?
C21 N4 C20 112.0(12) . . ?
C21 N4 Ta 125.8(10) . . ?
C20 N4 Ta 122.2(10) . . ?
C23 N5 C22 108.9(12) . . ?
C23 N5 Ta 125.7(10) . . ?
C22 N5 Ta 125.4(9) . . ?
C24 N6 C25 106.1(12) . . ?
C24 N6 Ta 127.0(10) . . ?
C25 N6 Ta 126.8(9) . . ?
C6 C1 C2 111.4(12) . . ?
C1 C2 C3 112.1(13) . . ?
C4 C3 C2 111.1(13) . . ?
C5 C4 C3 110.8(13) . . ?
C4 C5 C6 112.2(12) . . ?
N1 C6 C1 111.5(11) . . ?
N1 C6 C5 112.3(11) . . ?
C1 C6 C5 109.9(11) . . ?
C12 C7 C8 111.8(12) . . ?
C7 C8 C9 110.1(13) . . ?
C10 C9 C8 111.1(13) . . ?
C9 C10 C11 111.9(13) . . ?
C12 C11 C10 111.5(12) . . ?
N2 C12 C11 113.2(12) . . ?
N2 C12 C7 107.1(11) . . ?
C11 C12 C7 110.1(11) . . ?
C14 C13 C18 111.8(12) . . ?
C13 C14 C15 112.6(14) . . ?
C16 C15 C14 108.3(13) . . ?
C17 C16 C15 112.7(13) . . ?
C16 C17 C18 111.0(12) . . ?
N3 C18 C17 111.0(11) . . ?
N3 C18 C13 113.4(11) . . ?
C17 C18 C13 108.7(11) . . ?
N2 C19 N3 137.7(14) . . ?
N2 C19 N1 121.5(12) . . ?
N3 C19 N1 100.6(11) . . ?
N2 C19 Ta 164.6(11) . . ?
N3 C19 Ta 52.7(7) . . ?
N1 C19 Ta 49.0(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta N4 1.963(11) . ?
Ta N6 1.967(13) . ?
Ta N5 1.976(11) . ?
Ta N1 2.023(11) . ?
Ta N3 2.120(12) . ?
Ta C19 2.65(2) . ?
N1 C19 1.44(2) . ?
N1 C6 1.46(2) . ?
N2 C19 1.28(2) . ?
N2 C12 1.46(2) . ?
N3 C19 1.40(2) . ?
N3 C18 1.46(2) . ?
N4 C21 1.45(2) . ?
N4 C20 1.48(2) . ?
N5 C23 1.44(2) . ?
N5 C22 1.50(2) . ?
N6 C24 1.49(2) . ?
N6 C25 1.49(2) . ?
C1 C6 1.51(2) . ?
C1 C2 1.51(2) . ?
C2 C3 1.52(2) . ?
C3 C4 1.53(2) . ?
C4 C5 1.52(2) . ?
C5 C6 1.53(2) . ?
C7 C12 1.54(2) . ?
C7 C8 1.54(2) . ?
C8 C9 1.56(2) . ?
C9 C10 1.51(2) . ?
C10 C11 1.53(2) . ?
C11 C12 1.52(2) . ?
C13 C14 1.48(2) . ?
C13 C18 1.53(2) . ?
C14 C15 1.54(2) . ?
C15 C16 1.54(2) . ?
C16 C17 1.52(2) . ?
C17 C18 1.53(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30661135
