#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/17/7011739.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_7011739
loop_
_publ_author_name
'Boss, Sally R.'
'Haigh, Robert'
'Linton, David J.'
'Wheatley, Andrew E. H.'
_publ_section_title
;
 Oxygen scavenging by lithium zincates: the synthesis, structural
 characterisation and derivatisation of [Ph(2-C5H4N)N]2ZnRLi??nthf (R =
 But, Bun; n = 1, 2)
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3129
_journal_paper_doi               10.1039/b203451d
_journal_year                    2002
_chemical_formula_sum            'C30 H35 Li N4 O2 Zn'
_chemical_formula_weight         555.93
_chemical_name_common            aw0118
_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                107.10(3)
_cell_angle_beta                 106.27(3)
_cell_angle_gamma                111.01(3)
_cell_formula_units_Z            2
_cell_length_a                   11.715(2)
_cell_length_b                   12.228(2)
_cell_length_c                   12.323(3)
_cell_measurement_reflns_used    9559
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1420.4(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16302
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  1.075
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995) '
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0462
_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)+(0.0440P)²+0.3787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                4686
_reflns_number_total             6373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203451d.txt
_cod_data_source_block           aw0118
_cod_original_cell_volume        1420.3(9)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30 H35 Li1 N4 O2 Zn1'
_cod_database_code               7011739
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
Zn1 Zn -0.07969(3) 0.51168(3) -0.42701(2) 0.02220(11) Uani 1 1 d . . .
Li1 Li -0.0548(5) 0.6619(4) -0.5757(4) 0.0291(10) Uani 1 1 d . . .
O1 O -0.10027(16) 0.48604(16) -0.60311(14) 0.0217(4) Uani 1 1 d . . .
O2 O -0.0942(2) 0.70075(19) -0.72171(17) 0.0404(5) Uani 1 1 d . . .
N1 N -0.1526(2) 0.7229(2) -0.47486(19) 0.0269(5) Uani 1 1 d . . .
N2 N -0.0538(2) 0.6799(2) -0.31324(18) 0.0246(5) Uani 1 1 d . . .
N4 N -0.2160(2) 0.3608(2) -0.42551(18) 0.0242(5) Uani 1 1 d . . .
N3 N -0.1531(2) 0.2201(2) -0.53168(19) 0.0259(5) Uani 1 1 d . . .
C16 C -0.2497(3) 0.2363(2) -0.4999(2) 0.0230(6) Uani 1 1 d . . .
C17 C -0.2968(3) 0.3800(2) -0.3628(2) 0.0256(6) Uani 1 1 d . . .
C12 C -0.1870(3) 0.1014(3) -0.6160(2) 0.0312(6) Uani 1 1 d . . .
H12A H -0.1192 0.0912 -0.6389 0.037 Uiso 1 1 calc R . .
C21 C -0.4242(3) 0.4862(3) -0.3081(3) 0.0444(8) Uani 1 1 d . . .
H21A H -0.4623 0.5412 -0.3185 0.053 Uiso 1 1 calc R . .
C18 C -0.3117(3) 0.3278(3) -0.2778(2) 0.0324(7) Uani 1 1 d . . .
H18A H -0.2730 0.2733 -0.2666 0.039 Uiso 1 1 calc R . .
C1 C -0.2305(3) 0.7710(3) -0.5237(3) 0.0344(7) Uani 1 1 d . . .
H1A H -0.2494 0.7598 -0.6075 0.041 Uiso 1 1 calc R . .
C14 C -0.4106(3) 0.0091(3) -0.6355(3) 0.0362(7) Uani 1 1 d . . .
H14A H -0.4983 -0.0633 -0.6702 0.043 Uiso 1 1 calc R . .
C2 C -0.2840(3) 0.8343(3) -0.4611(3) 0.0390(7) Uani 1 1 d . . .
H2A H -0.3380 0.8666 -0.4995 0.047 Uiso 1 1 calc R . .
C23 C -0.2178(3) 0.3758(3) -0.7115(2) 0.0269(6) Uani 1 1 d . . .
H23A H -0.2219 0.2946 -0.7084 0.032 Uiso 1 1 calc R . .
H23B H -0.2079 0.3764 -0.7886 0.032 Uiso 1 1 calc R . .
C8 C 0.1071(3) 0.6923(3) -0.0017(2) 0.0370(7) Uani 1 1 d . . .
H8A H 0.1076 0.6330 0.0336 0.044 Uiso 1 1 calc R . .
C22 C -0.3546(3) 0.4590(3) -0.3767(3) 0.0332(7) Uani 1 1 d . . .
H22A H -0.3462 0.4950 -0.4345 0.040 Uiso 1 1 calc R . .
C24 C -0.3486(3) 0.3750(3) -0.7200(2) 0.0340(7) Uani 1 1 d . . .
H24A H -0.3481 0.4520 -0.7312 0.041 Uiso 1 1 calc R . .
H24B H -0.3545 0.3827 -0.6397 0.041 Uiso 1 1 calc R . .
C20 C -0.4388(3) 0.4339(3) -0.2246(3) 0.0467(8) Uani 1 1 d . . .
H20A H -0.4873 0.4522 -0.1778 0.056 Uiso 1 1 calc R . .
C3 C -0.2563(3) 0.8497(3) -0.3389(3) 0.0412(8) Uani 1 1 d . . .
H3A H -0.2921 0.8929 -0.2920 0.049 Uiso 1 1 calc R . .
C9 C 0.1895(3) 0.8243(3) 0.0729(3) 0.0458(8) Uani 1 1 d . . .
H9A H 0.2466 0.8562 0.1593 0.055 Uiso 1 1 calc R . .
C27 C -0.1679(5) 0.6206(4) -0.8511(3) 0.0824(15) Uani 1 1 d . . .
H27A H -0.2582 0.5535 -0.8691 0.099 Uiso 1 1 calc R . .
H27B H -0.1197 0.5756 -0.8813 0.099 Uiso 1 1 calc R . .
C10 C 0.1880(4) 0.9093(3) 0.0207(3) 0.0532(9) Uani 1 1 d . . .
H10A H 0.2442 1.0006 0.0716 0.064 Uiso 1 1 calc R . .
C19 C -0.3822(3) 0.3547(3) -0.2095(3) 0.0427(8) Uani 1 1 d . . .
H19A H -0.3917 0.3185 -0.1521 0.051 Uiso 1 1 calc R . .
C25 C -0.4736(3) 0.2521(3) -0.8278(3) 0.0544(9) Uani 1 1 d . . .
H25A H -0.4734 0.1755 -0.8159 0.065 Uiso 1 1 calc R . .
H25B H -0.5553 0.2552 -0.8228 0.065 Uiso 1 1 calc R . .
C11 C 0.1053(3) 0.8630(3) -0.1050(3) 0.0428(8) Uani 1 1 d . . .
H11A H 0.1055 0.9231 -0.1394 0.051 Uiso 1 1 calc R . .
C29 C -0.0898(4) 0.8381(4) -0.8207(3) 0.0594(10) Uani 1 1 d . . .
H29A H -0.1409 0.8846 -0.8016 0.071 Uiso 1 1 calc R . .
H29B H -0.0270 0.8849 -0.8506 0.071 Uiso 1 1 calc R . .
C30 C -0.0137(4) 0.8284(3) -0.7067(3) 0.0656(11) Uani 1 1 d . . .
H30A H 0.0765 0.8411 -0.7011 0.079 Uiso 1 1 calc R . .
H30B H -0.0009 0.8956 -0.6291 0.079 Uiso 1 1 calc R . .
C28 C -0.1838(5) 0.7008(4) -0.9164(4) 0.0762(13) Uani 1 1 d . . .
H28A H -0.2785 0.6850 -0.9487 0.091 Uiso 1 1 calc R . .
H28B H -0.1596 0.6805 -0.9880 0.091 Uiso 1 1 calc R . .
C26 C -0.4844(4) 0.2323(5) -0.9556(3) 0.0888(15) Uani 1 1 d . . .
H26A H -0.5662 0.1504 -1.0183 0.133 Uiso 1 1 calc R . .
H26B H -0.4044 0.2284 -0.9623 0.133 Uiso 1 1 calc R . .
H26C H -0.4898 0.3050 -0.9706 0.133 Uiso 1 1 calc R . .
C13 C -0.3125(3) -0.0056(3) -0.6711(3) 0.0363(7) Uani 1 1 d . . .
H13A H -0.3318 -0.0870 -0.7314 0.044 Uiso 1 1 calc R . .
C15 C -0.3806(3) 0.1281(3) -0.5505(2) 0.0319(6) Uani 1 1 d . . .
H15A H -0.4472 0.1384 -0.5254 0.038 Uiso 1 1 calc R . .
C7 C 0.0237(3) 0.6451(3) -0.1275(2) 0.0294(6) Uani 1 1 d . . .
H7A H -0.0331 0.5537 -0.1772 0.035 Uiso 1 1 calc R . .
C6 C 0.0213(3) 0.7288(3) -0.1829(2) 0.0260(6) Uani 1 1 d . . .
C4 C -0.1779(3) 0.8028(3) -0.2858(3) 0.0367(7) Uani 1 1 d . . .
H4A H -0.1587 0.8138 -0.2020 0.044 Uiso 1 1 calc R . .
C5 C -0.1254(3) 0.7379(2) -0.3556(2) 0.0242(6) Uani 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'
O O 0.0106 0.0060 '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'
Li Li -0.0003 0.0001 '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
N4 Zn1 N2 112.66(9) . . ?
N4 Zn1 O1 114.38(8) . 2_564 ?
N2 Zn1 O1 111.03(9) . 2_564 ?
N4 Zn1 O1 112.99(9) . . ?
N2 Zn1 O1 117.10(8) . . ?
O1 Zn1 O1 86.16(7) 2_564 . ?
N4 Zn1 Li1 140.25(11) . . ?
N2 Zn1 Li1 77.38(11) . . ?
O1 Zn1 Li1 95.17(10) 2_564 . ?
O1 Zn1 Li1 40.14(10) . . ?
N4 Zn1 Zn1 123.36(7) . 2_564 ?
N2 Zn1 Zn1 123.89(7) . 2_564 ?
O1 Zn1 Zn1 43.15(5) 2_564 2_564 ?
O1 Zn1 Zn1 43.01(5) . 2_564 ?
Li1 Zn1 Zn1 62.46(9) . 2_564 ?
N4 Zn1 Li1 77.93(11) . 2_564 ?
N2 Zn1 Li1 138.51(10) . 2_564 ?
O1 Zn1 Li1 37.67(10) 2_564 2_564 ?
O1 Zn1 Li1 91.70(9) . 2_564 ?
Li1 Zn1 Li1 121.07(8) . 2_564 ?
Zn1 Zn1 Li1 58.61(8) 2_564 2_564 ?
O1 Li1 O2 119.1(2) . . ?
O1 Li1 N1 107.9(2) . . ?
O2 Li1 N1 107.6(2) . . ?
O1 Li1 N3 108.9(2) . 2_564 ?
O2 Li1 N3 104.4(2) . 2_564 ?
N1 Li1 N3 108.6(2) . 2_564 ?
O1 Li1 Zn1 43.07(10) . . ?
O2 Li1 Zn1 159.2(2) . . ?
N1 Li1 Zn1 75.56(14) . . ?
N3 Li1 Zn1 93.64(16) 2_564 . ?
O1 Li1 Zn1 40.22(10) . 2_564 ?
O2 Li1 Zn1 117.1(2) . 2_564 ?
N1 Li1 Zn1 134.08(19) . 2_564 ?
N3 Li1 Zn1 71.14(14) 2_564 2_564 ?
Zn1 Li1 Zn1 58.93(8) . 2_564 ?
C23 O1 Li1 121.83(19) . . ?
C23 O1 Zn1 116.77(14) . 2_564 ?
Li1 O1 Zn1 102.11(16) . 2_564 ?
C23 O1 Zn1 120.22(15) . . ?
Li1 O1 Zn1 96.79(15) . . ?
Zn1 O1 Zn1 93.84(7) 2_564 . ?
C27 O2 C30 106.7(2) . . ?
C27 O2 Li1 132.3(2) . . ?
C30 O2 Li1 119.2(2) . . ?
C1 N1 C5 118.2(2) . . ?
C1 N1 Li1 116.9(2) . . ?
C5 N1 Li1 123.9(2) . . ?
C5 N2 C6 118.9(2) . . ?
C5 N2 Zn1 121.40(16) . . ?
C6 N2 Zn1 118.74(16) . . ?
C16 N4 C17 118.5(2) . . ?
C16 N4 Zn1 121.24(17) . . ?
C17 N4 Zn1 119.41(16) . . ?
C12 N3 C16 118.2(2) . . ?
C12 N3 Li1 113.2(2) . 2_564 ?
C16 N3 Li1 125.4(2) . 2_564 ?
N3 C16 N4 116.4(2) . . ?
N3 C16 C15 119.9(2) . . ?
N4 C16 C15 123.5(2) . . ?
C22 C17 C18 118.1(3) . . ?
C22 C17 N4 121.0(2) . . ?
C18 C17 N4 120.7(2) . . ?
N3 C12 C13 124.5(3) . . ?
C22 C21 C20 120.4(3) . . ?
C19 C18 C17 120.6(3) . . ?
N1 C1 C2 124.5(3) . . ?
C15 C14 C13 119.9(3) . . ?
C1 C2 C3 117.3(3) . . ?
O1 C23 C24 113.4(2) . . ?
C9 C8 C7 120.7(3) . . ?
C21 C22 C17 121.1(3) . . ?
C23 C24 C25 113.2(2) . . ?
C21 C20 C19 119.4(3) . . ?
C4 C3 C2 120.1(3) . . ?
C8 C9 C10 119.2(3) . . ?
O2 C27 C28 109.1(3) . . ?
C9 C10 C11 120.5(3) . . ?
C20 C19 C18 120.4(3) . . ?
C26 C25 C24 115.3(3) . . ?
C10 C11 C6 121.2(3) . . ?
C28 C29 C30 104.8(3) . . ?
O2 C30 C29 106.2(3) . . ?
C27 C28 C29 105.5(3) . . ?
C12 C13 C14 117.5(3) . . ?
C14 C15 C16 119.8(3) . . ?
C8 C7 C6 121.3(3) . . ?
C7 C6 C11 117.1(2) . . ?
C7 C6 N2 121.0(2) . . ?
C11 C6 N2 121.7(2) . . ?
C3 C4 C5 120.0(3) . . ?
N1 C5 N2 116.1(2) . . ?
N1 C5 C4 119.8(2) . . ?
N2 C5 C4 124.0(2) . . ?
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 N4 1.969(2) . ?
Zn1 N2 1.976(2) . ?
Zn1 O1 2.0239(17) 2_564 ?
Zn1 O1 2.0293(16) . ?
Zn1 Li1 2.951(4) . ?
Zn1 Zn1 2.9605(9) 2_564 ?
Zn1 Li1 3.065(5) 2_564 ?
Li1 O1 1.916(5) . ?
Li1 O2 1.968(5) . ?
Li1 N1 2.068(5) . ?
Li1 N3 2.077(5) 2_564 ?
Li1 Zn1 3.065(5) 2_564 ?
O1 C23 1.441(3) . ?
O1 Zn1 2.0239(17) 2_564 ?
O2 C27 1.397(4) . ?
O2 C30 1.427(4) . ?
N1 C1 1.352(3) . ?
N1 C5 1.354(3) . ?
N2 C5 1.371(3) . ?
N2 C6 1.406(3) . ?
N4 C16 1.364(3) . ?
N4 C17 1.417(3) . ?
N3 C12 1.346(3) . ?
N3 C16 1.356(3) . ?
N3 Li1 2.077(5) 2_564 ?
C16 C15 1.419(4) . ?
C17 C22 1.387(4) . ?
C17 C18 1.398(4) . ?
C12 C13 1.369(4) . ?
C21 C22 1.380(4) . ?
C21 C20 1.380(5) . ?
C18 C19 1.386(4) . ?
C1 C2 1.361(4) . ?
C14 C15 1.367(4) . ?
C14 C13 1.389(4) . ?
C2 C3 1.387(4) . ?
C23 C24 1.502(4) . ?
C8 C9 1.376(4) . ?
C8 C7 1.383(4) . ?
C24 C25 1.525(4) . ?
C20 C19 1.381(4) . ?
C3 C4 1.364(4) . ?
C9 C10 1.377(4) . ?
C27 C28 1.468(5) . ?
C10 C11 1.382(4) . ?
C25 C26 1.481(5) . ?
C11 C6 1.403(4) . ?
C29 C28 1.485(5) . ?
C29 C30 1.501(4) . ?
C7 C6 1.391(4) . ?
C4 C5 1.411(4) . ?
