#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:18:11 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179684 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/06/7000678.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_7000678
loop_
_publ_author_name
'Zhang, Jie'
'Han, Fuyan'
'Han, Yanan'
'Chen, Zhenxia'
'Zhou, Xigeng'
_publ_section_title
;
 Synthesis and structures of titanium and yttrium complexes with
 N,N′-tetramethylguanidinate ligands: different reactivity of
 the M--N bonds toward phenyl isocyanate
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              1806
_journal_page_last               1811
_journal_paper_doi               10.1039/b817776g
_journal_year                    2009
_chemical_formula_sum            'C26 H35 N4 O2 Y'
_chemical_formula_weight         524.49
_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                97.490(5)
_cell_angle_beta                 92.561(5)
_cell_angle_gamma                99.995(4)
_cell_formula_units_Z            2
_cell_length_a                   8.832(3)
_cell_length_b                   10.901(4)
_cell_length_c                   13.927(5)
_cell_measurement_reflns_used    729
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.617
_cell_measurement_theta_min      2.686
_cell_volume                     1306.1(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      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6036
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        3.23
_exptl_absorpt_coefficient_mu    2.261
_exptl_absorpt_correction_T_max  0.8055
_exptl_absorpt_correction_T_min  0.6606
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5033
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0549
_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/[σ²(Fo²)+(0.0886P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                3790
_reflns_number_total             5033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b817776g.txt
_cod_data_source_block           f40524a
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000678
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
Y1 Y 1.07093(5) 1.09179(4) 0.12717(3) 0.03915(17) Uani 1 1 d . . .
O1 O 0.9165(3) 0.9100(2) 0.03603(19) 0.0421(7) Uani 1 1 d . . .
N1 N 0.8935(4) 0.9327(3) 0.1925(2) 0.0410(8) Uani 1 1 d . . .
N2 N 0.7282(4) 0.7660(3) 0.0860(2) 0.0438(8) Uani 1 1 d . . .
N3 N 0.5509(5) 0.6134(4) 0.1388(3) 0.0587(11) Uani 1 1 d . . .
N4 N 0.8089(5) 0.6283(4) 0.1875(3) 0.0586(10) Uani 1 1 d . . .
C1 C 1.0712(11) 1.3168(7) 0.2245(7) 0.108(3) Uani 1 1 d . . .
H1A H 1.1556 1.3661 0.2689 0.129 Uiso 1 1 calc R . .
C2 C 1.0460(9) 1.3296(5) 0.1290(6) 0.087(2) Uani 1 1 d . . .
H2A H 1.1099 1.3897 0.0943 0.104 Uiso 1 1 calc R . .
C3 C 0.9037(8) 1.2674(6) 0.0980(5) 0.0767(17) Uani 1 1 d . . .
H3A H 0.8501 1.2732 0.0360 0.092 Uiso 1 1 calc R . .
C4 C 0.8357(8) 1.2120(5) 0.1725(7) 0.089(2) Uani 1 1 d . . .
H4A H 0.7272 1.1731 0.1732 0.107 Uiso 1 1 calc R . .
C5 C 0.9431(13) 1.2419(7) 0.2515(5) 0.102(3) Uani 1 1 d . . .
H5A H 0.9222 1.2287 0.3182 0.123 Uiso 1 1 calc R . .
C6 C 1.3464(8) 1.1572(8) 0.2239(7) 0.101(2) Uani 1 1 d . . .
H6A H 1.3820 1.2381 0.2650 0.121 Uiso 1 1 calc R . .
C7 C 1.3790(6) 1.1328(7) 0.1323(6) 0.0809(19) Uani 1 1 d . . .
H7A H 1.4426 1.1917 0.0965 0.097 Uiso 1 1 calc R . .
C8 C 1.3338(7) 1.0080(8) 0.1025(5) 0.088(2) Uani 1 1 d . . .
H8A H 1.3619 0.9602 0.0434 0.106 Uiso 1 1 calc R . .
C9 C 1.2699(7) 0.9572(6) 0.1850(8) 0.101(3) Uani 1 1 d . . .
H9A H 1.2472 0.8680 0.1930 0.121 Uiso 1 1 calc R . .
C10 C 1.2817(8) 1.0555(11) 0.2560(5) 0.099(3) Uani 1 1 d . . .
H10A H 1.2651 1.0487 0.3243 0.119 Uiso 1 1 calc R . .
C11 C 0.8444(5) 0.8662(4) 0.1080(3) 0.0392(9) Uani 1 1 d . . .
C12 C 0.6994(5) 0.6746(4) 0.1388(3) 0.0485(11) Uani 1 1 d . . .
C13 C 0.9683(6) 0.6512(5) 0.1638(5) 0.0727(16) Uani 1 1 d . . .
H13A H 0.9757 0.6865 0.1041 0.109 Uiso 1 1 calc R . .
H13B H 1.0062 0.5734 0.1565 0.109 Uiso 1 1 calc R . .
H13C H 1.0287 0.7090 0.2149 0.109 Uiso 1 1 calc R . .
C14 C 0.7818(8) 0.5752(5) 0.2769(4) 0.0843(19) Uani 1 1 d . . .
H14A H 0.6737 0.5626 0.2868 0.126 Uiso 1 1 calc R . .
H14B H 0.8376 0.6319 0.3304 0.126 Uiso 1 1 calc R . .
H14C H 0.8163 0.4960 0.2726 0.126 Uiso 1 1 calc R . .
C15 C 0.4263(7) 0.6744(6) 0.1115(5) 0.0806(17) Uani 1 1 d . . .
H15A H 0.4643 0.7627 0.1126 0.121 Uiso 1 1 calc R . .
H15B H 0.3474 0.6630 0.1564 0.121 Uiso 1 1 calc R . .
H15C H 0.3843 0.6382 0.0473 0.121 Uiso 1 1 calc R . .
C16 C 0.5108(8) 0.4783(5) 0.1405(5) 0.0832(18) Uani 1 1 d . . .
H16A H 0.6009 0.4469 0.1598 0.125 Uiso 1 1 calc R . .
H16B H 0.4715 0.4370 0.0769 0.125 Uiso 1 1 calc R . .
H16C H 0.4336 0.4619 0.1859 0.125 Uiso 1 1 calc R . .
C17 C 0.8176(5) 0.9155(4) 0.2787(3) 0.0439(10) Uani 1 1 d . . .
C18 C 0.8992(6) 0.8980(5) 0.3597(3) 0.0601(13) Uani 1 1 d . . .
H18A H 1.0030 0.8931 0.3569 0.072 Uiso 1 1 calc R . .
C19 C 0.8289(7) 0.8875(6) 0.4469(4) 0.0748(16) Uani 1 1 d . . .
H19A H 0.8853 0.8745 0.5015 0.090 Uiso 1 1 calc R . .
C20 C 0.6769(8) 0.8964(6) 0.4517(4) 0.0822(18) Uani 1 1 d . . .
H20A H 0.6294 0.8896 0.5095 0.099 Uiso 1 1 calc R . .
C21 C 0.5955(7) 0.9153(7) 0.3714(4) 0.0822(18) Uani 1 1 d . . .
H21A H 0.4919 0.9210 0.3745 0.099 Uiso 1 1 calc R . .
C22 C 0.6647(6) 0.9261(5) 0.2857(4) 0.0596(13) Uani 1 1 d . . .
H22A H 0.6080 0.9408 0.2318 0.072 Uiso 1 1 calc R . .
O2 O 0.285(3) 0.5308(17) 0.4802(17) 0.463(15) Uani 1 1 d D . .
C23 C 0.338(2) 0.572(2) 0.3966(15) 0.278(11) Uani 1 1 d D . .
H23A H 0.3205 0.5054 0.3421 0.333 Uiso 1 1 calc R . .
H23B H 0.4463 0.6098 0.4049 0.333 Uiso 1 1 calc R . .
C24 C 0.239(2) 0.668(2) 0.3850(11) 0.289(14) Uani 1 1 d D . .
H24A H 0.2920 0.7335 0.3509 0.346 Uiso 1 1 calc R . .
H24B H 0.1431 0.6295 0.3486 0.346 Uiso 1 1 calc R . .
C25 C 0.212(2) 0.7194(15) 0.4803(15) 0.255(9) Uani 1 1 d D . .
H25A H 0.1025 0.7072 0.4894 0.306 Uiso 1 1 calc R . .
H25B H 0.2543 0.8087 0.4928 0.306 Uiso 1 1 calc R . .
C26 C 0.288(3) 0.652(2) 0.5427(8) 0.288(11) Uani 1 1 d D . .
H26A H 0.2334 0.6405 0.6006 0.346 Uiso 1 1 calc R . .
H26B H 0.3934 0.6947 0.5616 0.346 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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
O1 Y1 O1 67.37(11) 2_775 . ?
O1 Y1 N1 121.09(11) 2_775 . ?
O1 Y1 N1 54.06(10) . . ?
O1 Y1 C2 84.63(19) 2_775 . ?
O1 Y1 C2 128.6(2) . . ?
N1 Y1 C2 126.20(17) . . ?
O1 Y1 C9 107.7(3) 2_775 . ?
O1 Y1 C9 91.3(2) . . ?
N1 Y1 C9 81.09(17) . . ?
C2 Y1 C9 139.3(2) . . ?
O1 Y1 C10 128.91(18) 2_775 . ?
O1 Y1 C10 117.2(3) . . ?
N1 Y1 C10 86.8(2) . . ?
C2 Y1 C10 114.0(3) . . ?
C9 Y1 C10 29.5(2) . . ?
O1 Y1 C1 114.0(3) 2_775 . ?
O1 Y1 C1 145.3(2) . . ?
N1 Y1 C1 110.5(3) . . ?
C2 Y1 C1 30.0(2) . . ?
C9 Y1 C1 118.7(3) . . ?
C10 Y1 C1 89.5(3) . . ?
O1 Y1 C5 128.52(18) 2_775 . ?
O1 Y1 C5 119.9(3) . . ?
N1 Y1 C5 81.3(2) . . ?
C2 Y1 C5 49.6(2) . . ?
C9 Y1 C5 122.0(3) . . ?
C10 Y1 C5 94.9(3) . . ?
C1 Y1 C5 30.1(2) . . ?
O1 Y1 C8 80.03(17) 2_775 . ?
O1 Y1 C8 94.24(18) . . ?
N1 Y1 C8 108.1(2) . . ?
C2 Y1 C8 123.4(3) . . ?
C9 Y1 C8 31.4(2) . . ?
C10 Y1 C8 49.5(2) . . ?
C1 Y1 C8 120.4(3) . . ?
C5 Y1 C8 140.9(3) . . ?
O1 Y1 C6 112.8(2) 2_775 . ?
O1 Y1 C6 138.59(19) . . ?
N1 Y1 C6 114.5(2) . . ?
C2 Y1 C6 91.4(3) . . ?
C9 Y1 C6 48.0(2) . . ?
C10 Y1 C6 28.3(2) . . ?
C1 Y1 C6 74.9(2) . . ?
C5 Y1 C6 93.0(3) . . ?
C8 Y1 C6 48.2(2) . . ?
O1 Y1 C3 79.60(16) 2_775 . ?
O1 Y1 C3 101.02(17) . . ?
N1 Y1 C3 104.14(18) . . ?
C2 Y1 C3 29.31(19) . . ?
C9 Y1 C3 167.5(3) . . ?
C10 Y1 C3 138.3(3) . . ?
C1 Y1 C3 48.8(2) . . ?
C5 Y1 C3 49.1(2) . . ?
C8 Y1 C3 147.4(3) . . ?
C6 Y1 C3 120.1(2) . . ?
O1 Y1 C7 84.93(18) 2_775 . ?
O1 Y1 C7 122.26(19) . . ?
N1 Y1 C7 130.04(15) . . ?
C2 Y1 C7 95.5(2) . . ?
C9 Y1 C7 49.31(18) . . ?
C10 Y1 C7 47.9(2) . . ?
C1 Y1 C7 91.8(3) . . ?
C5 Y1 C7 117.0(3) . . ?
C8 Y1 C7 29.4(2) . . ?
C6 Y1 C7 28.7(2) . . ?
C3 Y1 C7 123.3(2) . . ?
C11 O1 Y1 148.4(3) . 2_775 ?
C11 O1 Y1 97.7(2) . . ?
Y1 O1 Y1 112.63(11) 2_775 . ?
C11 N1 C17 122.9(4) . . ?
C11 N1 Y1 95.3(2) . . ?
C17 N1 Y1 139.6(3) . . ?
C12 N2 C11 124.0(4) . . ?
C12 N3 C15 119.5(4) . . ?
C12 N3 C16 122.7(5) . . ?
C15 N3 C16 115.9(5) . . ?
C12 N4 C13 121.2(4) . . ?
C12 N4 C14 122.8(5) . . ?
C13 N4 C14 115.0(5) . . ?
C2 C1 C5 107.9(7) . . ?
C2 C1 Y1 74.8(3) . . ?
C5 C1 Y1 75.3(4) . . ?
C3 C2 C1 108.2(7) . . ?
C3 C2 Y1 76.8(3) . . ?
C1 C2 Y1 75.2(4) . . ?
C2 C3 C4 109.5(6) . . ?
C2 C3 Y1 73.9(3) . . ?
C4 C3 Y1 76.2(3) . . ?
C3 C4 C5 106.4(6) . . ?
C3 C4 Y1 74.1(3) . . ?
C5 C4 Y1 73.1(3) . . ?
C1 C5 C4 107.9(7) . . ?
C1 C5 Y1 74.6(4) . . ?
C4 C5 Y1 76.9(3) . . ?
C10 C6 C7 111.0(7) . . ?
C10 C6 Y1 74.9(4) . . ?
C7 C6 Y1 76.2(4) . . ?
C6 C7 C8 108.5(7) . . ?
C6 C7 Y1 75.2(4) . . ?
C8 C7 Y1 74.6(3) . . ?
C7 C8 C9 105.3(6) . . ?
C7 C8 Y1 76.0(3) . . ?
C9 C8 Y1 73.5(3) . . ?
C10 C9 C8 105.9(6) . . ?
C10 C9 Y1 75.3(4) . . ?
C8 C9 Y1 75.0(3) . . ?
C6 C10 C9 109.3(7) . . ?
C6 C10 Y1 76.8(4) . . ?
C9 C10 Y1 75.1(4) . . ?
O1 C11 N1 112.8(4) . . ?
O1 C11 N2 117.6(4) . . ?
N1 C11 N2 129.5(4) . . ?
O1 C11 Y1 55.38(19) . . ?
N1 C11 Y1 57.5(2) . . ?
N2 C11 Y1 170.7(3) . . ?
N2 C12 N4 124.7(4) . . ?
N2 C12 N3 118.3(4) . . ?
N4 C12 N3 116.8(4) . . ?
C18 C17 C22 118.4(4) . . ?
C18 C17 N1 119.8(4) . . ?
C22 C17 N1 121.6(4) . . ?
C17 C18 C19 120.8(5) . . ?
C20 C19 C18 119.8(5) . . ?
C21 C20 C19 119.6(5) . . ?
C20 C21 C22 120.7(6) . . ?
C21 C22 C17 120.7(5) . . ?
C23 O2 C26 100.6(12) . . ?
O2 C23 C24 100.3(11) . . ?
C25 C24 C23 106.1(9) . . ?
C24 C25 C26 104.8(9) . . ?
C25 C26 O2 101.9(11) . . ?
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
Y1 O1 2.278(3) 2_775 ?
Y1 O1 2.377(3) . ?
Y1 N1 2.426(3) . ?
Y1 C2 2.637(6) . ?
Y1 C9 2.640(5) . ?
Y1 C10 2.642(6) . ?
Y1 C1 2.643(6) . ?
Y1 C5 2.651(6) . ?
Y1 C8 2.659(5) . ?
Y1 C6 2.664(6) . ?
Y1 C3 2.673(5) . ?
Y1 C7 2.676(6) . ?
O1 C11 1.309(5) . ?
O1 Y1 2.278(3) 2_775 ?
N1 C11 1.312(5) . ?
N1 C17 1.420(5) . ?
N2 C12 1.311(5) . ?
N2 C11 1.355(5) . ?
N3 C12 1.364(6) . ?
N3 C15 1.443(7) . ?
N3 C16 1.457(6) . ?
N4 C12 1.360(6) . ?
N4 C13 1.448(7) . ?
N4 C14 1.452(6) . ?
C1 C2 1.368(10) . ?
C1 C5 1.373(11) . ?
C2 C3 1.344(9) . ?
C3 C4 1.376(9) . ?
C4 C5 1.386(10) . ?
C6 C10 1.298(11) . ?
C6 C7 1.323(10) . ?
C7 C8 1.353(9) . ?
C8 C9 1.436(10) . ?
C9 C10 1.346(11) . ?
C17 C18 1.363(6) . ?
C17 C22 1.382(7) . ?
C18 C19 1.397(7) . ?
C19 C20 1.367(8) . ?
C20 C21 1.360(8) . ?
C21 C22 1.374(7) . ?
O2 C23 1.376(15) . ?
O2 C26 1.480(15) . ?
C23 C24 1.488(15) . ?
C24 C25 1.419(14) . ?
C25 C26 1.427(14) . ?
