# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Sjoerd Harder'
_publ_contact_author_email       SJOERD.HARDER@UNI-DUE.DE

_publ_section_title              
;
Convenient Synthesis and Crystal Structure of a
Monomeric Zinc Hydride Complex with a Three-Fold Coordinated Metal Center
;
_publ_author_name                'Sjoerd Harder'

# Attachment 'hasj185.cif'

data_hasj185
_database_code_depnum_ccdc_archive 'CCDC 724884'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            DIPPnacnacZnH
_chemical_melting_point          '211 C'
_chemical_formula_moiety         'C29 H42 N2 Zn'
_chemical_formula_sum            'C29 H42 N2 Zn'
_chemical_formula_weight         484.02

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.639(3)
_cell_length_b                   15.856(3)
_cell_length_c                   14.020(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.528(10)
_cell_angle_gamma                90.00
_cell_volume                     2707.1(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1040
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50265
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         30.50
_reflns_number_total             7976
_reflns_number_gt                6843
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.7776P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7976
_refine_ls_number_parameters     457
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0777
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Zn1 Zn 0.850247(11) 0.100467(8) 0.242712(9) 0.01624(5) Uani 1 1 d . . .
N1 N 0.80115(8) 0.17808(6) 0.32992(6) 0.01421(17) Uani 1 1 d . . .
N2 N 0.86865(8) 0.18361(6) 0.14578(6) 0.01404(17) Uani 1 1 d . . .
C1 C 0.75005(12) 0.31552(8) 0.38337(9) 0.0237(2) Uani 1 1 d . . .
C2 C 0.79051(9) 0.26083(7) 0.31266(7) 0.0153(2) Uani 1 1 d . . .
C3 C 0.81377(10) 0.30101(7) 0.23139(8) 0.0159(2) Uani 1 1 d . . .
C4 C 0.85071(9) 0.26578(7) 0.15390(7) 0.01441(19) Uani 1 1 d . . .
C5 C 0.87049(11) 0.32550(7) 0.07640(8) 0.0202(2) Uani 1 1 d . . .
C6 C 0.77787(9) 0.14212(6) 0.41671(7) 0.01438(19) Uani 1 1 d . . .
C7 C 0.86337(9) 0.13524(7) 0.50491(8) 0.0165(2) Uani 1 1 d . . .
C8 C 0.84315(11) 0.08970(8) 0.58376(8) 0.0205(2) Uani 1 1 d . . .
C9 C 0.74149(10) 0.05319(7) 0.57647(8) 0.0217(2) Uani 1 1 d . . .
C10 C 0.65676(10) 0.06371(7) 0.49067(8) 0.0198(2) Uani 1 1 d . . .
C11 C 0.67278(10) 0.10845(7) 0.40976(8) 0.0160(2) Uani 1 1 d . . .
C12 C 0.97496(10) 0.17575(8) 0.51458(8) 0.0204(2) Uani 1 1 d . . .
C13 C 1.01390(13) 0.22646(11) 0.61070(11) 0.0338(3) Uani 1 1 d . . .
C14 C 1.06078(12) 0.11015(10) 0.50649(13) 0.0334(3) Uani 1 1 d . . .
C15 C 0.57854(10) 0.12014(8) 0.31713(8) 0.0206(2) Uani 1 1 d . . .
C16 C 0.47432(12) 0.15211(12) 0.34163(12) 0.0373(3) Uani 1 1 d . . .
C17 C 0.55600(17) 0.03959(11) 0.25615(12) 0.0433(4) Uani 1 1 d . . .
C18 C 0.90562(9) 0.15411(6) 0.06301(7) 0.01431(19) Uani 1 1 d . . .
C19 C 0.82735(10) 0.12821(7) -0.02400(8) 0.0171(2) Uani 1 1 d . . .
C20 C 0.86580(11) 0.09646(7) -0.10190(8) 0.0212(2) Uani 1 1 d . . .
C21 C 0.97734(11) 0.08767(7) -0.09274(9) 0.0221(2) Uani 1 1 d . . .
C22 C 1.05308(11) 0.11267(7) -0.00600(9) 0.0194(2) Uani 1 1 d . . .
C23 C 1.01886(9) 0.14828(7) 0.07219(8) 0.0159(2) Uani 1 1 d . . .
C24 C 0.70497(10) 0.13127(8) -0.03220(9) 0.0226(2) Uani 1 1 d . . .
C25 C 0.66454(14) 0.04421(11) -0.01027(13) 0.0395(4) Uani 1 1 d . . .
C26 C 0.63640(13) 0.16413(11) -0.13196(11) 0.0357(3) Uani 1 1 d . . .
C27 C 1.10284(9) 0.17971(7) 0.16477(8) 0.0174(2) Uani 1 1 d . . .
C28 C 1.19858(11) 0.22648(9) 0.14072(10) 0.0286(3) Uani 1 1 d . . .
C29 C 1.14652(13) 0.10800(8) 0.23774(10) 0.0272(3) Uani 1 1 d . . .
H15 H 0.5991(12) 0.1628(9) 0.2758(10) 0.020(3) Uiso 1 1 d . . .
H10 H 0.5867(13) 0.0401(10) 0.4854(11) 0.024(4) Uiso 1 1 d . . .
H27 H 1.0671(12) 0.2183(9) 0.1982(10) 0.018(3) Uiso 1 1 d . . .
H22 H 1.1266(14) 0.1066(9) 0.0005(11) 0.021(4) Uiso 1 1 d . . .
H12 H 0.9693(12) 0.2146(10) 0.4599(11) 0.025(4) Uiso 1 1 d . . .
H21 H 1.0029(13) 0.0629(11) -0.1430(12) 0.030(4) Uiso 1 1 d . . .
H3 H 0.8038(13) 0.3606(10) 0.2291(11) 0.025(4) Uiso 1 1 d . . .
H20 H 0.8129(13) 0.0814(10) -0.1641(12) 0.023(4) Uiso 1 1 d . . .
H8 H 0.9001(15) 0.0850(11) 0.6454(13) 0.035(5) Uiso 1 1 d . . .
H24 H 0.6943(13) 0.1705(10) 0.0155(11) 0.027(4) Uiso 1 1 d . . .
H28A H 1.2449(14) 0.2535(11) 0.2011(12) 0.030(4) Uiso 1 1 d . . .
H5B H 0.8347(14) 0.3060(10) 0.0118(12) 0.030(4) Uiso 1 1 d . . .
H9 H 0.7273(12) 0.0218(10) 0.6303(11) 0.025(4) Uiso 1 1 d . . .
H13A H 1.0821(14) 0.2557(11) 0.6144(12) 0.031(4) Uiso 1 1 d . . .
H29A H 1.0915(14) 0.0785(11) 0.2557(12) 0.028(4) Uiso 1 1 d . . .
H5C H 0.9482(15) 0.3256(11) 0.0789(12) 0.033(4) Uiso 1 1 d . . .
H5A H 0.8443(13) 0.3816(11) 0.0828(12) 0.027(4) Uiso 1 1 d . . .
H1A H 0.8012(17) 0.3148(13) 0.4458(16) 0.055(6) Uiso 1 1 d . . .
H14A H 1.1268(17) 0.1371(13) 0.5081(14) 0.047(5) Uiso 1 1 d . . .
H16A H 0.4183(16) 0.1607(12) 0.2796(15) 0.048(5) Uiso 1 1 d . . .
H1C H 0.7335(15) 0.3730(12) 0.3588(13) 0.039(5) Uiso 1 1 d . . .
H28C H 1.1744(16) 0.2708(12) 0.0919(14) 0.047(5) Uiso 1 1 d . . .
H29C H 1.1868(14) 0.0672(11) 0.2088(12) 0.031(4) Uiso 1 1 d . . .
H26B H 0.6398(16) 0.1308(13) -0.1865(15) 0.045(5) Uiso 1 1 d . . .
H1B H 0.6860(17) 0.2933(13) 0.3949(14) 0.047(5) Uiso 1 1 d . . .
H14B H 1.0402(15) 0.0765(12) 0.4471(14) 0.038(5) Uiso 1 1 d . . .
H29B H 1.1959(15) 0.1276(12) 0.2970(14) 0.037(4) Uiso 1 1 d . . .
H17C H 0.619(2) 0.0229(16) 0.2352(18) 0.075(8) Uiso 1 1 d . . .
H13B H 1.0278(15) 0.1890(12) 0.6672(14) 0.042(5) Uiso 1 1 d . . .
H16B H 0.4427(16) 0.1106(12) 0.3783(15) 0.045(5) Uiso 1 1 d . . .
H28B H 1.2455(16) 0.1860(12) 0.1162(14) 0.044(5) Uiso 1 1 d . . .
H13C H 0.9575(16) 0.2678(12) 0.6147(14) 0.045(5) Uiso 1 1 d . . .
H25A H 0.7040(16) 0.0244(12) 0.0560(15) 0.048(5) Uiso 1 1 d . . .
H26C H 0.6603(16) 0.2198(13) -0.1485(14) 0.047(5) Uiso 1 1 d . . .
H17B H 0.5040(18) 0.0506(14) 0.1929(16) 0.059(6) Uiso 1 1 d . . .
H17A H 0.5297(15) -0.0043(12) 0.2942(14) 0.043(5) Uiso 1 1 d . . .
H26A H 0.5582(17) 0.1693(12) -0.1322(13) 0.045(5) Uiso 1 1 d . . .
H25C H 0.6732(17) 0.0050(14) -0.0610(16) 0.058(6) Uiso 1 1 d . . .
H25B H 0.5864(18) 0.0438(13) -0.0088(15) 0.055(6) Uiso 1 1 d . . .
H100 H 0.8662(14) 0.0091(12) 0.2472(12) 0.042(5) Uiso 1 1 d . . .
H14C H 1.0760(16) 0.0689(13) 0.5655(15) 0.048(5) Uiso 1 1 d . . .
H16C H 0.4875(19) 0.2012(16) 0.3851(17) 0.068(7) Uiso 1 1 d . . .

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
Zn1 0.02310(9) 0.01313(7) 0.01448(7) 0.00012(4) 0.00848(5) 0.00078(5)
N1 0.0156(4) 0.0155(4) 0.0122(4) 0.0005(3) 0.0048(3) 0.0002(3)
N2 0.0155(4) 0.0156(4) 0.0121(4) -0.0006(3) 0.0054(3) -0.0002(3)
C1 0.0343(7) 0.0191(5) 0.0221(5) -0.0011(4) 0.0154(5) 0.0050(5)
C2 0.0149(5) 0.0162(5) 0.0151(4) -0.0021(4) 0.0047(4) 0.0006(4)
C3 0.0180(5) 0.0130(4) 0.0176(4) 0.0001(4) 0.0064(4) 0.0013(4)
C4 0.0127(5) 0.0161(5) 0.0139(4) 0.0016(3) 0.0025(4) -0.0007(4)
C5 0.0255(6) 0.0175(5) 0.0201(5) 0.0044(4) 0.0104(4) 0.0010(4)
C6 0.0167(5) 0.0146(4) 0.0127(4) 0.0004(3) 0.0053(4) 0.0011(4)
C7 0.0164(5) 0.0184(5) 0.0143(4) -0.0009(4) 0.0037(4) 0.0016(4)
C8 0.0218(6) 0.0242(5) 0.0144(4) 0.0036(4) 0.0029(4) 0.0032(4)
C9 0.0264(6) 0.0217(5) 0.0180(5) 0.0057(4) 0.0079(4) 0.0014(5)
C10 0.0201(6) 0.0204(5) 0.0203(5) 0.0026(4) 0.0078(4) -0.0023(4)
C11 0.0164(5) 0.0167(5) 0.0148(4) 0.0006(3) 0.0041(4) 0.0007(4)
C12 0.0169(6) 0.0256(6) 0.0176(5) -0.0014(4) 0.0026(4) -0.0027(4)
C13 0.0260(7) 0.0454(8) 0.0290(6) -0.0141(6) 0.0055(5) -0.0105(6)
C14 0.0181(7) 0.0397(8) 0.0440(8) -0.0059(6) 0.0110(6) 0.0002(6)
C15 0.0162(6) 0.0261(5) 0.0174(5) 0.0040(4) 0.0008(4) -0.0019(4)
C16 0.0176(7) 0.0591(10) 0.0343(7) 0.0122(7) 0.0052(6) 0.0083(7)
C17 0.0470(10) 0.0387(8) 0.0318(7) -0.0094(6) -0.0110(7) -0.0027(7)
C18 0.0184(5) 0.0133(4) 0.0123(4) 0.0009(3) 0.0061(4) -0.0002(4)
C19 0.0202(6) 0.0164(5) 0.0143(4) 0.0002(4) 0.0040(4) 0.0000(4)
C20 0.0285(7) 0.0200(5) 0.0146(4) -0.0027(4) 0.0050(4) -0.0005(4)
C21 0.0319(7) 0.0203(5) 0.0180(5) -0.0017(4) 0.0132(5) 0.0010(5)
C22 0.0214(6) 0.0193(5) 0.0210(5) 0.0014(4) 0.0119(4) 0.0005(4)
C23 0.0185(5) 0.0145(4) 0.0154(4) 0.0017(3) 0.0059(4) -0.0003(4)
C24 0.0186(6) 0.0287(6) 0.0186(5) -0.0028(4) 0.0015(4) -0.0006(5)
C25 0.0265(8) 0.0460(9) 0.0434(8) 0.0099(7) 0.0049(6) -0.0116(7)
C26 0.0270(8) 0.0456(9) 0.0284(6) 0.0058(6) -0.0031(6) 0.0053(6)
C27 0.0159(5) 0.0182(5) 0.0182(5) 0.0002(4) 0.0049(4) -0.0002(4)
C28 0.0221(6) 0.0350(7) 0.0270(6) 0.0054(5) 0.0034(5) -0.0094(5)
C29 0.0327(8) 0.0241(6) 0.0205(5) 0.0044(4) -0.0006(5) -0.0033(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Zn1 N1 1.9495(9) . ?
Zn1 N2 1.9515(9) . ?
N1 C2 1.3345(14) . ?
N1 C6 1.4436(13) . ?
N2 C4 1.3325(14) . ?
N2 C18 1.4402(13) . ?
C1 C2 1.5058(15) . ?
C2 C3 1.4036(15) . ?
C3 C4 1.4077(15) . ?
C4 C5 1.5117(15) . ?
C6 C11 1.4105(16) . ?
C6 C7 1.4118(15) . ?
C7 C8 1.3999(15) . ?
C7 C12 1.5226(17) . ?
C8 C9 1.3879(18) . ?
C9 C10 1.3899(17) . ?
C10 C11 1.3977(15) . ?
C11 C15 1.5204(15) . ?
C12 C14 1.5289(19) . ?
C12 C13 1.5327(17) . ?
C15 C17 1.521(2) . ?
C15 C16 1.5337(19) . ?
C18 C23 1.4053(16) . ?
C18 C19 1.4104(15) . ?
C19 C20 1.4024(16) . ?
C19 C24 1.5210(17) . ?
C20 C21 1.3880(19) . ?
C21 C22 1.3889(17) . ?
C22 C23 1.4005(15) . ?
C23 C27 1.5239(15) . ?
C24 C26 1.5262(18) . ?
C24 C25 1.531(2) . ?
C27 C29 1.5303(17) . ?
C27 C28 1.5318(17) . ?

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
N1 Zn1 N2 97.33(4) . . ?
C2 N1 C6 120.52(9) . . ?
C2 N1 Zn1 122.71(7) . . ?
C6 N1 Zn1 116.76(7) . . ?
C4 N2 C18 119.06(9) . . ?
C4 N2 Zn1 123.11(7) . . ?
C18 N2 Zn1 117.81(7) . . ?
N1 C2 C3 124.10(9) . . ?
N1 C2 C1 118.83(9) . . ?
C3 C2 C1 117.06(10) . . ?
C2 C3 C4 129.14(10) . . ?
N2 C4 C3 123.58(9) . . ?
N2 C4 C5 119.10(9) . . ?
C3 C4 C5 117.32(10) . . ?
C11 C6 C7 121.14(10) . . ?
C11 C6 N1 119.47(9) . . ?
C7 C6 N1 119.19(10) . . ?
C8 C7 C6 118.21(11) . . ?
C8 C7 C12 120.53(10) . . ?
C6 C7 C12 121.27(10) . . ?
C9 C8 C7 121.21(10) . . ?
C8 C9 C10 119.82(10) . . ?
C9 C10 C11 121.19(11) . . ?
C10 C11 C6 118.31(10) . . ?
C10 C11 C15 120.30(10) . . ?
C6 C11 C15 121.38(10) . . ?
C7 C12 C14 111.41(11) . . ?
C7 C12 C13 111.80(10) . . ?
C14 C12 C13 110.79(12) . . ?
C11 C15 C17 111.33(11) . . ?
C11 C15 C16 111.87(10) . . ?
C17 C15 C16 111.13(13) . . ?
C23 C18 C19 121.42(10) . . ?
C23 C18 N2 119.32(9) . . ?
C19 C18 N2 119.19(10) . . ?
C20 C19 C18 117.97(11) . . ?
C20 C19 C24 120.67(10) . . ?
C18 C19 C24 121.32(10) . . ?
C21 C20 C19 121.27(11) . . ?
C20 C21 C22 119.82(11) . . ?
C21 C22 C23 121.03(12) . . ?
C22 C23 C18 118.38(10) . . ?
C22 C23 C27 120.52(10) . . ?
C18 C23 C27 121.10(9) . . ?
C19 C24 C26 113.37(11) . . ?
C19 C24 C25 110.08(11) . . ?
C26 C24 C25 110.71(12) . . ?
C23 C27 C29 111.77(10) . . ?
C23 C27 C28 112.46(9) . . ?
C29 C27 C28 110.00(11) . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.052