#------------------------------------------------------------------------------
#$Date: 2025-08-20 15:06:16 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301830 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/78/4077803.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_4077803
loop_
_publ_author_name
'Morton, Colin'
'Munslow, Ian J.'
'Sanders, Christopher J.'
'Alcock, Nathaniel W.'
'Scott, Peter'
_publ_section_title
;
 Triamidoamine Chemistry of Zirconium
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4608
_journal_paper_doi               10.1021/om990347e
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C26 H63 N5 Si3 Zr'
_chemical_formula_weight         621.30
_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
_cell_angle_alpha                106.48
_cell_angle_beta                 103.5540(10)
_cell_angle_gamma                95.8210(10)
_cell_formula_units_Z            2
_cell_length_a                   9.69980(10)
_cell_length_b                   13.1685(3)
_cell_length_c                   15.2304(4)
_cell_measurement_reflns_used    5578
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1783.87(7)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10552
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       Block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.907
_refine_ls_goodness_of_fit_obs   0.945
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         7706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_restrained_S_obs      0.945
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_obs          0.0450
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0515P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1082
_refine_ls_wR_factor_obs         0.0929
_reflns_number_observed          5321
_reflns_number_total             7706
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990347e.cif
_cod_data_source_block
'chi_compound_2_in_Scott_and_co-workers_Triamidoamine chemistry....'
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1783.89(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077803
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Zr1 Zr 0.21985(3) 0.19233(2) 0.80035(2) 0.02161(9) Uani 1 d .
Si1 Si 0.09978(9) 0.22432(7) 1.00110(6) 0.0241(2) Uani 1 d .
Si2 Si 0.35639(9) -0.04984(7) 0.78661(6) 0.0256(2) Uani 1 d .
Si3 Si 0.21004(11) 0.37700(7) 0.67434(7) 0.0334(2) Uani 1 d .
N1 N 0.0887(2) 0.24063(19) 0.89041(17) 0.0228(6) Uani 1 d .
N2 N -0.0324(3) 0.1048(2) 0.70159(18) 0.0252(6) Uani 1 d .
N3 N 0.2180(2) 0.02439(19) 0.77389(18) 0.0249(6) Uani 1 d .
N4 N 0.1805(3) 0.2464(2) 0.67947(17) 0.0265(6) Uani 1 d .
N5 N 0.4299(3) 0.2699(2) 0.86798(19) 0.0280(6) Uani 1 d .
C1 C 0.2343(4) 0.4410(3) 1.1072(3) 0.0522(11) Uani 1 d .
H1A H 0.2328 0.5086 1.1549 0.078 Uiso 1 calc R
H1B H 0.2227 0.4522 1.0451 0.078 Uiso 1 calc R
H1C H 0.3264 0.4177 1.1258 0.078 Uiso 1 calc R
C2 C 0.1348(5) 0.3329(3) 1.1968(3) 0.0532(11) Uani 1 d .
H2A H 0.1421 0.4003 1.2474 0.080 Uiso 1 calc R
H2B H 0.2242 0.3044 1.2100 0.080 Uiso 1 calc R
H2C H 0.0536 0.2803 1.1942 0.080 Uiso 1 calc R
C3 C -0.0307(4) 0.3984(3) 1.0809(3) 0.0489(10) Uani 1 d .
H3A H -0.0229 0.4657 1.1317 0.073 Uiso 1 calc R
H3B H -0.1109 0.3455 1.0792 0.073 Uiso 1 calc R
H3C H -0.0481 0.4119 1.0195 0.073 Uiso 1 calc R
C4 C 0.1104(3) 0.3543(3) 1.1003(2) 0.0300(7) Uani 1 d .
C5 C -0.0618(4) 0.1281(3) 0.9952(2) 0.0381(9) Uani 1 d .
H5A H -0.1497 0.1557 0.9743 0.057 Uiso 1 calc R
H5B H -0.0545 0.1209 1.0583 0.057 Uiso 1 calc R
H5C H -0.0654 0.0576 0.9497 0.057 Uiso 1 calc R
C6 C 0.2626(3) 0.1630(3) 1.0338(2) 0.0356(8) Uani 1 d .
H6A H 0.3494 0.2122 1.0393 0.053 Uiso 1 calc R
H6B H 0.2547 0.0945 0.9844 0.053 Uiso 1 calc R
H6C H 0.2690 0.1504 1.0949 0.053 Uiso 1 calc R
C7 C -0.0576(3) 0.2486(3) 0.8360(2) 0.0288(7) Uani 1 d .
H7A H -0.0489 0.3033 0.8035 0.035 Uiso 1 calc R
H7B H -0.1175 0.2708 0.8801 0.035 Uiso 1 calc R
C8 C -0.1285(3) 0.1386(3) 0.7624(2) 0.0315(8) Uani 1 d .
H8A H -0.1447 0.0851 0.7950 0.038 Uiso 1 calc R
H8B H -0.2230 0.1434 0.7229 0.038 Uiso 1 calc R
C9 C -0.0336(3) -0.0123(2) 0.6727(2) 0.0323(8) Uani 1 d .
H9A H -0.0053 -0.0351 0.6127 0.039 Uiso 1 calc R
H9B H -0.1321 -0.0514 0.6613 0.039 Uiso 1 calc R
C10 C 0.0704(3) -0.0400(2) 0.7502(2) 0.0312(8) Uani 1 d .
H10A H 0.0357 -0.0250 0.8079 0.037 Uiso 1 calc R
H10B H 0.0744 -0.1177 0.7284 0.037 Uiso 1 calc R
C11 C 0.5252(3) 0.0349(3) 0.8756(2) 0.0376(9) Uani 1 d .
H11A H 0.5003 0.0866 0.9273 0.056 Uiso 1 calc R
H11B H 0.5791 0.0739 0.8445 0.056 Uiso 1 calc R
H11C H 0.5846 -0.0113 0.9016 0.056 Uiso 1 calc R
C12 C 0.3084(4) -0.1630(3) 0.8326(3) 0.0404(9) Uani 1 d .
H12A H 0.2876 -0.1337 0.8939 0.061 Uiso 1 calc R
H12B H 0.3893 -0.2015 0.8410 0.061 Uiso 1 calc R
H12C H 0.2231 -0.2128 0.7869 0.061 Uiso 1 calc R
C13 C 0.3980(3) -0.1118(3) 0.6682(2) 0.0323(8) Uani 1 d .
C14 C 0.4318(4) -0.0247(3) 0.6238(3) 0.0482(10) Uani 1 d .
H14A H 0.4504 -0.0581 0.5624 0.072 Uiso 1 calc R
H14B H 0.5172 0.0275 0.6666 0.072 Uiso 1 calc R
H14C H 0.3495 0.0123 0.6139 0.072 Uiso 1 calc R
C15 C 0.5294(4) -0.1686(3) 0.6841(3) 0.0499(11) Uani 1 d .
H15A H 0.5473 -0.2028 0.6227 0.075 Uiso 1 calc R
H15B H 0.5096 -0.2235 0.7137 0.075 Uiso 1 calc R
H15C H 0.6145 -0.1155 0.7259 0.075 Uiso 1 calc R
C16 C 0.2683(4) -0.1952(3) 0.5973(3) 0.0435(9) Uani 1 d .
H16A H 0.2912 -0.2253 0.5368 0.065 Uiso 1 calc R
H16B H 0.1841 -0.1604 0.5864 0.065 Uiso 1 calc R
H16C H 0.2471 -0.2531 0.6234 0.065 Uiso 1 calc R
C17 C -0.0650(3) 0.1418(3) 0.6171(2) 0.0334(8) Uani 1 d .
H17A H -0.1110 0.2062 0.6307 0.040 Uiso 1 calc R
H17B H -0.1326 0.0845 0.5624 0.040 Uiso 1 calc R
C18 C 0.0753(3) 0.1692(3) 0.5931(2) 0.0329(8) Uani 1 d .
H18A H 0.1146 0.1029 0.5714 0.039 Uiso 1 calc R
H18B H 0.0572 0.2015 0.5412 0.039 Uiso 1 calc R
C19 C 0.0322(4) 0.4213(3) 0.6383(3) 0.0513(11) Uani 1 d .
H19A H -0.0224 0.3746 0.5744 0.077 Uiso 1 calc R
H19B H 0.0497 0.4959 0.6383 0.077 Uiso 1 calc R
H19C H -0.0231 0.4165 0.6837 0.077 Uiso 1 calc R
C20 C 0.3085(4) 0.4702(3) 0.7961(2) 0.0406(9) Uani 1 d .
H20A H 0.4100 0.4622 0.8107 0.061 Uiso 1 calc R
H20B H 0.2651 0.4525 0.8431 0.061 Uiso 1 calc R
H20C H 0.3021 0.5446 0.7983 0.061 Uiso 1 calc R
C21 C 0.3145(5) 0.3957(3) 0.5856(3) 0.0457(10) Uani 1 d .
C22 C 0.2274(6) 0.3379(4) 0.4816(3) 0.0793(16) Uani 1 d .
H22A H 0.2784 0.3583 0.4390 0.119 Uiso 1 calc R
H22B H 0.1322 0.3586 0.4705 0.119 Uiso 1 calc R
H22C H 0.2161 0.2598 0.4690 0.119 Uiso 1 calc R
C23 C 0.4549(5) 0.3517(5) 0.6013(3) 0.0829(16) Uani 1 d .
H23A H 0.5090 0.3673 0.5583 0.124 Uiso 1 calc R
H23B H 0.4329 0.2737 0.5882 0.124 Uiso 1 calc R
H23C H 0.5129 0.3859 0.6675 0.124 Uiso 1 calc R
C24 C 0.3487(8) 0.5157(4) 0.5989(4) 0.117(3) Uani 1 d .
H24A H 0.3948 0.5262 0.5506 0.176 Uiso 1 calc R
H24B H 0.4140 0.5531 0.6625 0.176 Uiso 1 calc R
H24C H 0.2592 0.5450 0.5922 0.176 Uiso 1 calc R
C25 C 0.5043(4) 0.3379(3) 0.9648(3) 0.0430(9) Uani 1 d .
H25A H 0.5485 0.4077 0.9636 0.064 Uiso 1 calc R
H25B H 0.5793 0.3030 0.9931 0.064 Uiso 1 calc R
H25C H 0.4351 0.3489 1.0027 0.064 Uiso 1 calc R
C26 C 0.5298(4) 0.2638(3) 0.8090(3) 0.0427(9) Uani 1 d .
H26A H 0.5656 0.3363 0.8095 0.064 Uiso 1 calc R
H26B H 0.4796 0.2188 0.7435 0.064 Uiso 1 calc R
H26C H 0.6110 0.2321 0.8344 0.064 Uiso 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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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_publ_flag
N5 Zr1 N1 109.75(9) y
N5 Zr1 N4 99.96(10) y
N1 Zr1 N4 114.44(10) y
N5 Zr1 N3 107.11(10) y
N1 Zr1 N3 108.30(9) y
N4 Zr1 N3 116.62(10) y
N5 Zr1 N2 173.21(10) y
N1 Zr1 N2 74.75(8) y
N4 Zr1 N2 73.36(9) y
N3 Zr1 N2 75.53(9) y
N1 Si1 C6 107.99(14) ?
N1 Si1 C5 110.63(14) ?
C6 Si1 C5 107.31(16) ?
N1 Si1 C4 114.35(14) ?
C6 Si1 C4 109.55(15) ?
C5 Si1 C4 106.80(14) ?
N3 Si2 C11 111.45(13) ?
N3 Si2 C12 111.47(14) ?
C11 Si2 C12 105.63(17) ?
N3 Si2 C13 111.71(14) ?
C11 Si2 C13 108.87(15) ?
C12 Si2 C13 107.45(15) ?
N4 Si3 C20 108.84(15) ?
N4 Si3 C19 109.97(16) ?
C20 Si3 C19 107.04(17) ?
N4 Si3 C21 114.89(14) ?
C20 Si3 C21 109.23(17) ?
C19 Si3 C21 106.58(19) ?
C7 N1 Si1 115.59(19) ?
C7 N1 Zr1 111.66(18) ?
Si1 N1 Zr1 128.15(13) ?
C8 N2 C9 113.2(3) ?
C8 N2 C17 111.4(2) ?
C9 N2 C17 110.6(2) ?
C8 N2 Zr1 106.84(17) ?
C9 N2 Zr1 106.06(17) ?
C17 N2 Zr1 108.37(18) ?
C10 N3 Si2 114.04(19) ?
C10 N3 Zr1 113.39(18) ?
Si2 N3 Zr1 132.17(13) ?
C18 N4 Si3 113.7(2) ?
C18 N4 Zr1 114.30(19) ?
Si3 N4 Zr1 129.15(14) ?
C25 N5 C26 109.3(2) ?
C25 N5 Zr1 133.8(2) ?
C26 N5 Zr1 116.9(2) ?
C1 C4 C3 108.0(3) ?
C1 C4 C2 108.9(3) ?
C3 C4 C2 108.5(3) ?
C1 C4 Si1 110.9(2) ?
C3 C4 Si1 110.4(2) ?
C2 C4 Si1 110.1(2) ?
N1 C7 C8 108.8(2) ?
N2 C8 C7 108.6(2) ?
N2 C9 C10 110.0(3) ?
N3 C10 C9 110.6(3) ?
C14 C13 C16 108.2(3) ?
C14 C13 C15 108.8(3) ?
C16 C13 C15 108.5(3) ?
C14 C13 Si2 110.6(2) ?
C16 C13 Si2 110.7(2) ?
C15 C13 Si2 110.0(2) ?
N2 C17 C18 108.7(3) ?
N4 C18 C17 109.0(2) ?
C24 C21 C23 109.3(4) ?
C24 C21 C22 108.1(4) ?
C23 C21 C22 107.1(3) ?
C24 C21 Si3 108.4(3) ?
C23 C21 Si3 111.5(3) ?
C22 C21 Si3 112.4(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 N5 2.063(2) y
Zr1 N1 2.096(2) y
Zr1 N4 2.124(3) y
Zr1 N3 2.130(2) y
Zr1 N2 2.509(2) y
Si1 N1 1.739(3) ?
Si1 C6 1.874(3) ?
Si1 C5 1.880(3) ?
Si1 C4 1.910(3) ?
Si2 N3 1.746(3) ?
Si2 C11 1.869(3) ?
Si2 C12 1.880(4) ?
Si2 C13 1.911(3) ?
Si3 N4 1.742(3) ?
Si3 C20 1.871(3) ?
Si3 C19 1.887(4) ?
Si3 C21 1.922(4) ?
N1 C7 1.496(4) ?
N2 C8 1.476(4) ?
N2 C9 1.477(4) ?
N2 C17 1.479(4) ?
N3 C10 1.495(4) ?
N4 C18 1.486(4) ?
N5 C25 1.455(4) ?
N5 C26 1.460(4) ?
C1 C4 1.535(4) ?
C2 C4 1.542(5) ?
C3 C4 1.538(4) ?
C7 C8 1.532(4) ?
C9 C10 1.518(4) ?
C13 C14 1.533(5) ?
C13 C16 1.538(4) ?
C13 C15 1.548(4) ?
C17 C18 1.525(4) ?
C21 C24 1.527(6) ?
C21 C23 1.527(6) ?
C21 C22 1.536(6) ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139106787
