# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005 

data_global
_journal_coden_Cambridge         222
_journal_volume                  ?
_journal_year                    ?
_journal_page_first              ?

_publ_requested_journal          'Dalton Transactions'

loop_
_publ_author_name
T.A.Lowes
B.D.Ward
R.A.Whannel
S.R.Dubberley,
P.Mountford

_publ_contact_letter             
;
These are the CIF format data (1 compound) for the paper

A new diamido-amine ligand based on three-carbon atom "arms":
synthesis, structures and polymerisation capability of zirconium
derivatives of MeN(CH2CH2CH2NSiMe3)2

T. A. Lowes, B. D. Ward, R. A. Whannel, S. R. Dubberley, and
P. Mountford
;
_publ_contact_author             
;
Dr P. Mountford
Chemistry Research Laboratory
Mansfield Road
Oxford
OX1 3TA
UK
;

_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk

data_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 247514'
_audit_creation_method           CRYSTALS
#  Local code BDW8
_chemical_name_systematic        
;
[Zr{MeN(CH2CH2CH2NSiMe3)2}(CH2Ph)2]
;
_publ_section_exptl_refinement   
;
The refined Flack parameter of 0.50(3) is indicative of an
intimately twinned structure since Friedel pairs were collected
but not merged.
;
_cell_length_a                   20.9927(4)
_cell_length_b                   12.0115(2)
_cell_length_c                   12.1022(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3051.6(1)
_symmetry_cell_setting           'Orthorhombic '
_symmetry_space_group_name_H-M   'P n a 21 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,z
-x,-y,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C   ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H   ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997
0.0030 International_Tables_Vol_IV_Table_2.2B
'N   ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'Si  ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 International_Tables_Vol_IV_Table_2.2B
'Zr  ' -2.9650 0.5600 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572
87.6627 2.0693 International_Tables_Vol_IV_Table_2.2B
_chemical_formula_sum            ' C27 H47 N3 Si2 Zr1 '
_chemical_formula_moiety         ' C27 H47 N3 Si2 Zr1 '
_chemical_compound_source        
;
?
;
_chemical_formula_weight         561.09
_cell_measurement_reflns_used    3762
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485
_cell_measurement_temperature    150
_cell_formula_units_Z            4
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.20
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_max          0.70
_exptl_crystal_density_diffrn    1.22
_exptl_crystal_density_method    none
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_F_000             1180.68
_exptl_absorpt_coefficient_mu    0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_T_max  0.912
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_number         'not measured'
_diffrn_standards_decay_%        'not measured'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      150
_diffrn_reflns_number            6952
_reflns_number_total             6677
_diffrn_reflns_av_R_equivalents  0.00
_reflns_number_gt                5525
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.910
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              0
_reflns_limit_h_max              27
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              -15
_reflns_limit_l_max              15
_refine_diff_density_min         -0.55
_refine_diff_density_max         0.39
_reflns_threshold_expression     >3.00\s(I)
_refine_ls_number_reflns         5525
_refine_ls_number_parameters     299
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0262
_refine_ls_goodness_of_fit_ref   1.0850
_refine_ls_shift/su_max          0.003
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_abs_structure_details Flack
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979,
0.278    -.195E-010.146E-01
;
_refine_ls_hydrogen_treatment    'riding model'
_atom_sites_solution_primary     'direct methods'
_atom_sites_solution_hydrogens   geometric
_refine_ls_matrix_type           full
_refine_ls_number_restraints     0
_refine_ls_extinction_coef       147(11)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'

_computing_data_collection       
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction        
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement       
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_computing_structure_refinement  
;
CRYSTALS Issue 10 (Watkin et al., 1996)
;
_computing_molecular_graphics    'CAMERON (Watkin, Prout and Pearce, 1996)'

_computing_publication_material  
;
CRYSTALS Issue 10 (Watkin et al., 1996)
;

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
Zr1 0.704657(9) 0.164395(16) 0.97003(4) 0.0159 1.0000 Uani
N1 0.78487(9) 0.07643(17) 0.93267(17) 0.0210 1.0000 Uani
N2 0.6676(1) -0.02208(18) 1.03982(17) 0.0219 1.0000 Uani
N3 0.62807(9) 0.14207(17) 0.86694(17) 0.0194 1.0000 Uani
Si1 0.86326(3) 0.09635(5) 0.9743(1) 0.0252 1.0000 Uani
Si2 0.61337(3) 0.13186(6) 0.72673(7) 0.0205 1.0000 Uani
C1 0.77364(13) -0.0173(2) 0.8540(2) 0.0239 1.0000 Uani
C2 0.74552(13) -0.1197(2) 0.9093(2) 0.0263 1.0000 Uani
C3 0.67743(12) -0.1065(2) 0.9502(2) 0.0243 1.0000 Uani
C4 0.59876(13) -0.0220(2) 1.0706(2) 0.0280 1.0000 Uani
C5 0.55429(11) 0.0265(2) 0.9837(3) 0.0300 1.0000 Uani
C6 0.57424(12) 0.1435(2) 0.9459(2) 0.0259 1.0000 Uani
C7 0.91180(15) 0.1498(3) 0.8573(3) 0.0522 1.0000 Uani
C8 0.86541(16) 0.1975(3) 1.0905(3) 0.0491 1.0000 Uani
C9 0.90060(14) -0.0344(3) 1.0251(3) 0.0381 1.0000 Uani
C10 0.70355(15) -0.0581(2) 1.1391(2) 0.0284 1.0000 Uani
C11 0.60565(15) -0.0150(2) 0.6760(2) 0.0327 1.0000 Uani
C12 0.68130(13) 0.1968(2) 0.6515(2) 0.0274 1.0000 Uani
C13 0.53822(13) 0.2062(3) 0.6895(2) 0.0312 1.0000 Uani
C14 0.69954(12) 0.2255(2) 1.1516(2) 0.0221 1.0000 Uani
C15 0.64027(13) 0.2350(2) 1.2178(2) 0.0234 1.0000 Uani
C16 0.59212(13) 0.3114(2) 1.1891(2) 0.0293 1.0000 Uani
C17 0.53465(14) 0.3148(3) 1.2454(3) 0.0365 1.0000 Uani
C18 0.52307(16) 0.2423(3) 1.3327(3) 0.0422 1.0000 Uani
C19 0.57051(16) 0.1694(3) 1.3646(2) 0.0387 1.0000 Uani
C20 0.62839(14) 0.1666(2) 1.3089(2) 0.0304 1.0000 Uani
C21 0.73565(12) 0.3398(2) 0.9087(2) 0.0236 1.0000 Uani
C22 0.68907(12) 0.4279(2) 0.9404(2) 0.0223 1.0000 Uani
C23 0.70136(14) 0.5019(2) 1.0268(2) 0.0297 1.0000 Uani
C24 0.65666(15) 0.5781(2) 1.0635(3) 0.0344 1.0000 Uani
C25 0.59720(15) 0.5840(3) 1.0133(3) 0.0379 1.0000 Uani
C26 0.58429(15) 0.5136(3) 0.9255(3) 0.0376 1.0000 Uani
C27 0.62914(14) 0.4363(2) 0.8899(2) 0.0311 1.0000 Uani
H11 0.81490 -0.0376 0.8180 0.0300 1.0000 Uiso
H12 0.74276 0.0085 0.7965 0.0300 1.0000 Uiso
H21 0.77300 -0.1378 0.9744 0.0336 1.0000 Uiso
H22 0.74670 -0.1829 0.8555 0.0336 1.0000 Uiso
H31 0.66256 -0.1802 0.9787 0.0305 1.0000 Uiso
H32 0.65067 -0.0840 0.8856 0.0305 1.0000 Uiso
H41 0.59376 0.0237 1.1391 0.0378 1.0000 Uiso
H42 0.58550 -0.1005 1.0860 0.0378 1.0000 Uiso
H51 0.51016 0.0296 1.0146 0.0379 1.0000 Uiso
H52 0.55493 -0.0241 0.9180 0.0379 1.0000 Uiso
H61 0.58689 0.1878 1.0123 0.0322 1.0000 Uiso
H62 0.53693 0.1797 0.9092 0.0322 1.0000 Uiso
H71 0.95689 0.1611 0.8815 0.0650 1.0000 Uiso
H72 0.89370 0.2223 0.8314 0.0650 1.0000 Uiso
H73 0.91055 0.0946 0.7956 0.0650 1.0000 Uiso
H81 0.91055 0.2089 1.1144 0.0623 1.0000 Uiso
H82 0.84001 0.1675 1.1538 0.0623 1.0000 Uiso
H83 0.84693 0.2701 1.0660 0.0623 1.0000 Uiso
H91 0.94557 -0.0197 1.0481 0.0483 1.0000 Uiso
H92 0.87582 -0.0628 1.0897 0.0483 1.0000 Uiso
H93 0.90013 -0.0913 0.9647 0.0483 1.0000 Uiso
H101 0.69738 -0.0021 1.1992 0.0372 1.0000 Uiso
H102 0.74984 -0.0632 1.1202 0.0372 1.0000 Uiso
H103 0.68800 -0.1325 1.1646 0.0372 1.0000 Uiso
H111 0.59727 -0.0147 0.5947 0.0392 1.0000 Uiso
H112 0.64587 -0.0568 0.6914 0.0392 1.0000 Uiso
H113 0.56935 -0.0517 0.7152 0.0392 1.0000 Uiso
H121 0.67369 0.1917 0.5701 0.0343 1.0000 Uiso
H122 0.72164 0.1569 0.6706 0.0343 1.0000 Uiso
H123 0.68501 0.2768 0.6734 0.0343 1.0000 Uiso
H131 0.53043 0.1995 0.6083 0.0380 1.0000 Uiso
H132 0.54201 0.2866 0.7099 0.0380 1.0000 Uiso
H133 0.50188 0.1721 0.7308 0.0380 1.0000 Uiso
H141 0.72810 0.1746 1.1942 0.0310 1.0000 Uiso
H142 0.71816 0.3022 1.1509 0.0310 1.0000 Uiso
H161 0.59988 0.3656 1.1279 0.0365 1.0000 Uiso
H171 0.50061 0.3680 1.2220 0.0448 1.0000 Uiso
H181 0.48135 0.2434 1.3726 0.0502 1.0000 Uiso
H191 0.56298 0.1184 1.4287 0.0480 1.0000 Uiso
H201 0.66206 0.1136 1.3344 0.0396 1.0000 Uiso
H211 0.77798 0.3586 0.9417 0.0321 1.0000 Uiso
H212 0.73938 0.3382 0.8264 0.0321 1.0000 Uiso
H231 0.74374 0.4989 1.0644 0.0373 1.0000 Uiso
H241 0.66729 0.6295 1.1258 0.0425 1.0000 Uiso
H251 0.56466 0.6389 1.0393 0.0465 1.0000 Uiso
H261 0.54194 0.5170 0.8878 0.0470 1.0000 Uiso
H271 0.61861 0.3855 0.8270 0.0370 1.0000 Uiso
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.01508(8) 0.01600(9) 0.01672(9) -0.00104(14) 0.00047(13) -0.00046(8)
N1 0.017(1) 0.019(1) 0.0272(11) -0.0039(8) 0.0019(8) 0.0003(8)
N2 0.0244(11) 0.0220(11) 0.0192(11) -0.0008(8) 0.0022(8) -0.0021(9)
N3 0.017(1) 0.0205(11) 0.021(1) -0.0026(8) -0.0010(8) -0.0004(8)
Si1 0.0168(3) 0.0235(3) 0.0354(4) 0.0006(5) -0.0001(5) -0.0013(2)
Si2 0.0203(3) 0.0221(3) 0.0192(3) -0.0031(3) -0.0019(3) 0.0011(3)
C1 0.0251(13) 0.0219(13) 0.0248(13) -0.004(1) 0.003(1) 0.001(1)
C2 0.0312(14) 0.0202(13) 0.0275(14) -0.005(1) 0.0013(11) 0.0011(11)
C3 0.0297(12) 0.0199(11) 0.0232(17) -0.003(1) 0.003(1) -0.0063(9)
C4 0.0263(14) 0.0277(14) 0.0298(14) -0.0011(11) 0.0092(11) -0.0077(11)
C5 0.017(1) 0.0430(15) 0.0296(18) -0.0072(14) 0.0077(12) -0.007(1)
C6 0.0187(11) 0.0357(15) 0.0234(17) -0.007(1) 0.0013(9) 0.002(1)
C7 0.0265(16) 0.068(3) 0.062(2) 0.022(2) 0.0017(15) -0.0162(16)
C8 0.0335(17) 0.0448(19) 0.069(2) -0.0230(18) -0.0191(16) 0.0081(15)
C9 0.0253(15) 0.0338(17) 0.055(2) 0.0032(15) -0.0010(14) 0.0061(12)
C10 0.0397(15) 0.0236(13) 0.0219(12) 0.005(1) 0.0002(12) 0.0008(12)
C11 0.0408(17) 0.0303(15) 0.0271(14) -0.0087(12) -0.0050(12) -0.0026(13)
C12 0.0300(14) 0.0282(14) 0.0241(13) -0.0018(11) 0.0026(11) 0.0017(11)
C13 0.0253(14) 0.0439(16) 0.0245(14) -0.0050(12) -0.0035(11) 0.0054(12)
C14 0.0237(12) 0.0235(12) 0.0190(11) -0.0034(9) -0.000(1) 0.0002(11)
C15 0.0285(13) 0.0222(12) 0.0195(12) -0.007(1) 0.0013(11) -0.006(1)
C16 0.0307(14) 0.0294(15) 0.0277(14) -0.0100(11) -0.0007(11) 0.0000(11)
C17 0.0279(15) 0.0387(17) 0.0430(18) -0.0178(14) 0.0005(13) 0.0016(12)
C18 0.0371(17) 0.0474(19) 0.0422(19) -0.0183(15) 0.0161(14) -0.0119(15)
C19 0.0526(19) 0.0387(16) 0.0249(14) -0.0088(13) 0.0147(13) -0.0149(15)
C20 0.0427(17) 0.0306(14) 0.0179(12) -0.0053(12) 0.0032(11) -0.0049(13)
C21 0.0262(13) 0.0199(12) 0.0247(13) 0.001(1) 0.001(1) -0.0043(11)
C22 0.0263(13) 0.0153(12) 0.0253(15) 0.0054(9) -0.0016(9) -0.0040(9)
C23 0.0259(13) 0.0199(13) 0.0432(16) -0.0011(12) -0.0068(13) -0.0009(12)
C24 0.0375(16) 0.0219(14) 0.0439(17) -0.0049(13) -0.0026(13) 0.0003(12)
C25 0.0336(16) 0.0260(15) 0.0540(18) 0.0006(13) -0.0010(13) 0.0070(13)
C26 0.0308(16) 0.0311(16) 0.0509(18) 0.0055(14) -0.0135(13) 0.0023(13)
C27 0.0341(16) 0.0251(14) 0.0340(15) 0.0030(12) -0.0095(12) 0.0015(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 . N1 . 2.039(2) yes
Zr1 . N2 . 2.517(2) yes
Zr1 . N3 . 2.053(2) yes
Zr1 . C14 . 2.319(2) yes
Zr1 . C21 . 2.327(3) yes
N1 . Si1 . 1.738(2) yes
N1 . C1 . 1.493(3) yes
N2 . C3 . 1.499(3) yes
N2 . C4 . 1.492(3) yes
N2 . C10 . 1.483(3) yes
N3 . Si2 . 1.729(2) yes
N3 . C6 . 1.480(3) yes
Si1 . C7 . 1.859(3) yes
Si1 . C8 . 1.858(3) yes
Si1 . C9 . 1.860(3) yes
Si2 . C11 . 1.874(3) yes
Si2 . C12 . 1.863(3) yes
Si2 . C13 . 1.868(3) yes
C1 . C2 . 1.520(4) yes
C2 . C3 . 1.521(4) yes
C4 . C5 . 1.522(4) yes
C5 . C6 . 1.536(4) yes
C14 . C15 . 1.484(4) yes
C15 . C16 . 1.408(4) yes
C15 . C20 . 1.398(4) yes
C16 . C17 . 1.386(4) yes
C17 . C18 . 1.390(5) yes
C18 . C19 . 1.381(5) yes
C19 . C20 . 1.390(4) yes
C21 . C22 . 1.490(4) yes
C22 . C23 . 1.396(4) yes
C22 . C27 . 1.402(4) yes
C23 . C24 . 1.384(4) yes
C24 . C25 . 1.390(4) yes
C25 . C26 . 1.384(4) yes
C26 . C27 . 1.391(4) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Zr1 . N2 . 82.45(8) yes
N1 . Zr1 . N3 . 116.39(8) yes
N2 . Zr1 . N3 . 81.11(7) yes
N1 . Zr1 . C14 . 114.36(9) yes
N2 . Zr1 . C14 . 87.11(8) yes
N3 . Zr1 . C14 . 125.52(9) yes
N1 . Zr1 . C21 . 99.65(9) yes
N2 . Zr1 . C21 . 177.86(8) yes
N3 . Zr1 . C21 . 98.25(9) yes
C14 . Zr1 . C21 . 91.62(9) yes
Zr1 . N1 . Si1 . 130.28(11) yes
Zr1 . N1 . C1 . 113.68(15) yes
Si1 . N1 . C1 . 116.01(16) yes
Zr1 . N2 . C3 . 108.45(14) yes
Zr1 . N2 . C4 . 112.51(16) yes
C3 . N2 . C4 . 108.33(19) yes
Zr1 . N2 . C10 . 111.95(15) yes
C3 . N2 . C10 . 108.6(2) yes
C4 . N2 . C10 . 106.9(2) yes
Zr1 . N3 . Si2 . 138.21(12) yes
Zr1 . N3 . C6 . 101.79(15) yes
Si2 . N3 . C6 . 119.87(16) yes
N1 . Si1 . C7 . 110.21(14) yes
N1 . Si1 . C8 . 109.43(13) yes
C7 . Si1 . C8 . 109.70(19) yes
N1 . Si1 . C9 . 112.24(12) yes
C7 . Si1 . C9 . 108.20(16) yes
C8 . Si1 . C9 . 106.99(17) yes
N3 . Si2 . C11 . 113.79(12) yes
N3 . Si2 . C12 . 108.25(11) yes
C11 . Si2 . C12 . 107.47(13) yes
N3 . Si2 . C13 . 110.70(11) yes
C11 . Si2 . C13 . 107.33(14) yes
C12 . Si2 . C13 . 109.18(13) yes
N1 . C1 . C2 . 113.0(2) yes
C1 . C2 . C3 . 115.1(2) yes
N2 . C3 . C2 . 115.8(2) yes
N2 . C4 . C5 . 114.9(2) yes
C4 . C5 . C6 . 112.9(2) yes
N3 . C6 . C5 . 113.0(2) yes
Zr1 . C14 . C15 . 125.04(17) yes
C14 . C15 . C16 . 121.3(2) yes
C14 . C15 . C20 . 122.0(2) yes
C16 . C15 . C20 . 116.7(3) yes
C15 . C16 . C17 . 121.5(3) yes
C16 . C17 . C18 . 120.5(3) yes
C17 . C18 . C19 . 118.9(3) yes
C18 . C19 . C20 . 120.6(3) yes
C15 . C20 . C19 . 121.6(3) yes
Zr1 . C21 . C22 . 112.15(16) yes
C21 . C22 . C23 . 121.5(2) yes
C21 . C22 . C27 . 121.9(2) yes
C23 . C22 . C27 . 116.5(2) yes
C22 . C23 . C24 . 122.4(3) yes
C23 . C24 . C25 . 120.2(3) yes
C24 . C25 . C26 . 118.7(3) yes
C25 . C26 . C27 . 120.9(3) yes
C22 . C27 . C26 . 121.4(3) yes
#end