#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:37:28 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180148 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/45/7104535.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_7104535
loop_
_publ_author_name
'Spielmann, Jan'
'Piesik, Dirk'
'Wittkamp, Bernd'
'Jansen, Georg'
'Harder, Sjoerd'
_publ_section_title
;
 Convenient synthesis and crystal structure of a monomeric zinc hydride
 complex with a three-coordinate metal center.
;
_journal_issue                   23
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3455
_journal_page_last               3456
_journal_paper_doi               10.1039/b906319f
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C29 H42 N2 Zn'
_chemical_formula_sum            'C29 H42 N2 Zn'
_chemical_formula_weight         484.02
_chemical_melting_point          484.15
_chemical_name_common            DIPPnacnacZnH
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.528(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.639(3)
_cell_length_b                   15.856(3)
_cell_length_c                   14.020(3)
_cell_measurement_temperature    123(2)
_cell_volume                     2707.1(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50265
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0278
_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)+(0.0403P)²+0.7776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                6843
_reflns_number_total             7976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906319f.txt
_cod_data_source_block           hasj185
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '211 C' was changed to '484.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7104535
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'
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_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'
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) . . ?
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) . ?
