#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:23:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179841 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013799.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_7013799
loop_
_publ_author_name
'Dove, Andrew P.'
'Gibson, Vernon C.'
'Marshall, Edward L.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Magnesium and zinc complexes of a potentially tridentate
 beta-diketiminate ligand.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              570
_journal_page_last               578
_journal_paper_doi               10.1039/b314760f
_journal_year                    2004
_chemical_formula_sum            'C30 H49 N3 O Si2 Zn'
_chemical_formula_weight         589.27
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 104.289(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.407(2)
_cell_length_b                   18.2361(15)
_cell_length_c                   16.251(3)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      10.56
_cell_volume                     3275.9(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5132
_diffrn_reflns_theta_max         59.97
_diffrn_reflns_theta_min         3.71
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  0.7651
_exptl_absorpt_correction_T_min  0.3427
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00018(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.112
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.280
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_obs          0.0355
_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)+(0.0413P)²+2.9085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1059
_refine_ls_wR_factor_obs         0.0896
_reflns_number_observed          4456
_reflns_number_total             4859
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b314760f.txt
_cod_data_source_block           Compound_7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+2.9085P] 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^)+(0.0413P)^2^+2.9085P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7013799
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn Zn 0.85229(3) 0.18602(2) 0.74521(2) 0.02361(12) Uani 1 d . .
C1 C 0.8124(2) 0.23918(13) 0.90139(15) 0.0249(5) Uani 1 d . .
N1 N 0.7740(2) 0.19075(11) 0.83927(12) 0.0232(4) Uani 1 d . .
C2 C 0.8916(2) 0.29718(13) 0.89836(15) 0.0258(5) Uani 1 d . .
H2A H 0.9213(2) 0.32249(13) 0.95044(15) 0.031 Uiso 1 calc R .
C3 C 0.9336(2) 0.32335(13) 0.82976(15) 0.0234(5) Uani 1 d . .
N3 N 0.9243(2) 0.28478(11) 0.75918(12) 0.0243(4) Uani 1 d . .
C4 C 0.7656(3) 0.2347(2) 0.9805(2) 0.0382(7) Uani 1 d . .
H4A H 0.8062(3) 0.2717(2) 1.0214(2) 0.057 Uiso 1 d R .
H4B H 0.7820(3) 0.1858(2) 1.0056(2) 0.057 Uiso 1 d R .
H4C H 0.6782(3) 0.2437(2) 0.9656(2) 0.057 Uiso 1 d R .
C5 C 0.9849(3) 0.40013(14) 0.8392(2) 0.0352(6) Uani 1 d . .
H5A H 1.0735(3) 0.39771(14) 0.8528(2) 0.053 Uiso 1 d R .
H5B H 0.9594(3) 0.42544(14) 0.8851(2) 0.053 Uiso 1 d R .
H5C H 0.9552(3) 0.42705(14) 0.7860(2) 0.053 Uiso 1 d R .
C6 C 0.6712(2) 0.14486(13) 0.83962(15) 0.0234(5) Uani 1 d . .
C7 C 0.6879(2) 0.07116(13) 0.86363(15) 0.0252(5) Uani 1 d . .
C8 C 0.5856(2) 0.02690(15) 0.8551(2) 0.0322(6) Uani 1 d . .
H8A H 0.5951(2) -0.02328(15) 0.8711(2) 0.039 Uiso 1 calc R .
C9 C 0.4714(2) 0.05478(15) 0.8240(2) 0.0363(6) Uani 1 d . .
H9A H 0.4030(2) 0.02360(15) 0.8169(2) 0.044 Uiso 1 calc R .
C10 C 0.4562(2) 0.1280(2) 0.8031(2) 0.0352(6) Uani 1 d . .
H10A H 0.3767(2) 0.1469(2) 0.7826(2) 0.042 Uiso 1 calc R .
C11 C 0.5542(2) 0.17481(14) 0.8113(2) 0.0282(6) Uani 1 d . .
C12 C 0.8115(2) 0.03796(14) 0.9010(2) 0.0320(6) Uani 1 d . .
H12A H 0.8737(2) 0.07662(14) 0.9011(2) 0.038 Uiso 1 calc R .
C13 C 0.8375(3) -0.0265(2) 0.8484(2) 0.0443(7) Uani 1 d . .
H13A H 0.9179(3) -0.0465(2) 0.8745(2) 0.066 Uiso 1 calc R .
H13B H 0.8349(3) -0.0098(2) 0.7906(2) 0.066 Uiso 1 calc R .
H13C H 0.7764(3) -0.0647(2) 0.8462(2) 0.066 Uiso 1 calc R .
C14 C 0.8227(3) 0.0144(2) 0.9933(2) 0.0451(7) Uani 1 d . .
H14A H 0.9029(3) -0.0069(2) 1.0166(2) 0.068 Uiso 1 calc R .
H14B H 0.7604(3) -0.0221(2) 0.9950(2) 0.068 Uiso 1 calc R .
H14C H 0.8119(3) 0.0572(2) 1.0271(2) 0.068 Uiso 1 calc R .
C15 C 0.5323(2) 0.25582(15) 0.7905(2) 0.0365(6) Uani 1 d . .
H15A H 0.6114(2) 0.28209(15) 0.8096(2) 0.044 Uiso 1 calc R .
C16 C 0.4449(4) 0.2883(2) 0.8377(3) 0.0799(13) Uani 1 d . .
H16A H 0.4760(4) 0.2802(2) 0.8988(3) 0.120 Uiso 1 calc R .
H16B H 0.3657(4) 0.2646(2) 0.8183(3) 0.120 Uiso 1 calc R .
H16C H 0.4365(4) 0.3411(2) 0.8264(3) 0.120 Uiso 1 calc R .
C17 C 0.4857(5) 0.2679(2) 0.6966(2) 0.0865(14) Uani 1 d . .
H17A H 0.5427(5) 0.2468(2) 0.6668(2) 0.130 Uiso 1 calc R .
H17B H 0.4775(5) 0.3206(2) 0.6849(2) 0.130 Uiso 1 calc R .
H17C H 0.4067(5) 0.2442(2) 0.6769(2) 0.130 Uiso 1 calc R .
C18 C 0.9630(2) 0.31322(13) 0.6888(2) 0.0254(5) Uani 1 d . .
C19 C 0.8807(2) 0.31152(13) 0.6091(2) 0.0292(6) Uani 1 d . .
C20 C 0.9143(3) 0.33689(15) 0.5379(2) 0.0377(7) Uani 1 d . .
H20A H 0.8578(3) 0.33623(15) 0.4841(2) 0.045 Uiso 1 calc R .
C21 C 1.0299(3) 0.3631(2) 0.5450(2) 0.0409(7) Uani 1 d . .
H21A H 1.0522(3) 0.3812(2) 0.4962(2) 0.049 Uiso 1 calc R .
C22 C 1.1128(3) 0.3632(2) 0.6223(2) 0.0401(7) Uani 1 d . .
H22A H 1.1926(3) 0.3807(2) 0.6268(2) 0.048 Uiso 1 calc R .
C23 C 1.0800(2) 0.33774(14) 0.6938(2) 0.0326(6) Uani 1 d . .
H23A H 1.1382(2) 0.33703(14) 0.7469(2) 0.039 Uiso 1 calc R .
O24 O 0.7688(2) 0.28350(10) 0.60851(11) 0.0351(4) Uani 1 d . .
C25 C 0.6764(3) 0.2891(2) 0.5307(2) 0.0479(8) Uani 1 d . .
H25A H 0.6014(3) 0.2673(2) 0.5384(2) 0.072 Uiso 1 calc R .
H25B H 0.7024(3) 0.2630(2) 0.4855(2) 0.072 Uiso 1 calc R .
H25C H 0.6625(3) 0.3409(2) 0.5151(2) 0.072 Uiso 1 calc R .
N26 N 0.9010(2) 0.10806(11) 0.68437(12) 0.0260(5) Uani 1 d . .
Si27 Si 0.79964(6) 0.07010(4) 0.59976(5) 0.0333(2) Uani 1 d . .
C28 C 0.8225(3) 0.1042(2) 0.4961(2) 0.0649(11) Uani 1 d . .
H28A H 0.9046(3) 0.0920(2) 0.4920(2) 0.097 Uiso 1 calc R .
H28B H 0.8114(3) 0.1575(2) 0.4928(2) 0.097 Uiso 1 calc R .
H28C H 0.7636(3) 0.0809(2) 0.4493(2) 0.097 Uiso 1 calc R .
C29 C 0.6430(2) 0.0935(2) 0.6071(2) 0.0427(7) Uani 1 d . .
H29A H 0.6350(2) 0.1468(2) 0.6105(2) 0.064 Uiso 1 calc R .
H29B H 0.6273(2) 0.0707(2) 0.6580(2) 0.064 Uiso 1 calc R .
H29C H 0.5844(2) 0.0751(2) 0.5566(2) 0.064 Uiso 1 calc R .
C30 C 0.8088(3) -0.0322(2) 0.5934(2) 0.0601(10) Uani 1 d . .
H30A H 0.8901(3) -0.0464(2) 0.5895(2) 0.090 Uiso 1 calc R .
H30B H 0.7491(3) -0.0496(2) 0.5430(2) 0.090 Uiso 1 calc R .
H30C H 0.7920(3) -0.0540(2) 0.6444(2) 0.090 Uiso 1 calc R .
Si31 Si 1.05451(6) 0.09536(4) 0.71039(4) 0.0296(2) Uani 1 d . .
C32 C 1.1197(2) 0.1376(2) 0.8166(2) 0.0394(7) Uani 1 d . .
H32A H 1.0982(2) 0.1897(2) 0.8148(2) 0.059 Uiso 1 calc R .
H32B H 1.2079(2) 0.1325(2) 0.8310(2) 0.059 Uiso 1 calc R .
H32C H 1.0871(2) 0.1128(2) 0.8596(2) 0.059 Uiso 1 calc R .
C33 C 1.1301(3) 0.1372(2) 0.6317(2) 0.0514(8) Uani 1 d . .
H33A H 1.1082(3) 0.1891(2) 0.6241(2) 0.077 Uiso 1 calc R .
H33B H 1.1037(3) 0.1117(2) 0.5772(2) 0.077 Uiso 1 calc R .
H33C H 1.2181(3) 0.1326(2) 0.6526(2) 0.077 Uiso 1 calc R .
C34 C 1.1006(3) -0.0029(2) 0.7211(3) 0.0602(9) Uani 1 d . .
H34A H 1.0687(3) -0.0281(2) 0.6669(3) 0.090 Uiso 1 calc R .
H34B H 1.0683(3) -0.0260(2) 0.7652(3) 0.090 Uiso 1 calc R .
H34C H 1.1891(3) -0.0063(2) 0.7367(3) 0.090 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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
N26 Zn N1 133.80(9) . . ?
N26 Zn N3 125.42(8) . . ?
N1 Zn N3 97.34(8) . . ?
N1 C1 C2 124.7(2) . . ?
N1 C1 C4 119.3(2) . . ?
C2 C1 C4 116.0(2) . . ?
C1 N1 C6 119.8(2) . . ?
C1 N1 Zn 119.6(2) . . ?
C6 N1 Zn 120.46(15) . . ?
C1 C2 C3 129.5(2) . . ?
N3 C3 C2 122.5(2) . . ?
N3 C3 C5 121.7(2) . . ?
C2 C3 C5 115.8(2) . . ?
C3 N3 C18 121.9(2) . . ?
C3 N3 Zn 121.7(2) . . ?
C18 N3 Zn 116.4(2) . . ?
C7 C6 C11 121.0(2) . . ?
C7 C6 N1 120.3(2) . . ?
C11 C6 N1 118.6(2) . . ?
C8 C7 C6 118.3(2) . . ?
C8 C7 C12 118.7(2) . . ?
C6 C7 C12 123.0(2) . . ?
C9 C8 C7 121.0(2) . . ?
C8 C9 C10 120.0(2) . . ?
C9 C10 C11 121.5(2) . . ?
C10 C11 C6 118.0(2) . . ?
C10 C11 C15 119.5(2) . . ?
C6 C11 C15 122.6(2) . . ?
C7 C12 C13 111.9(2) . . ?
C7 C12 C14 110.4(2) . . ?
C13 C12 C14 110.6(2) . . ?
C17 C15 C16 110.1(3) . . ?
C17 C15 C11 111.4(3) . . ?
C16 C15 C11 111.0(2) . . ?
C23 C18 C19 118.4(2) . . ?
C23 C18 N3 123.7(2) . . ?
C19 C18 N3 117.8(2) . . ?
O24 C19 C20 124.5(2) . . ?
O24 C19 C18 115.2(2) . . ?
C20 C19 C18 120.3(2) . . ?
C21 C20 C19 120.1(3) . . ?
C22 C21 C20 120.3(3) . . ?
C21 C22 C23 119.9(3) . . ?
C22 C23 C18 120.9(3) . . ?
C19 O24 C25 117.3(2) . . ?
Si27 N26 Si31 126.23(12) . . ?
Si27 N26 Zn 119.83(11) . . ?
Si31 N26 Zn 112.75(11) . . ?
N26 Si27 C29 108.89(12) . . ?
N26 Si27 C30 114.34(14) . . ?
C29 Si27 C30 107.31(15) . . ?
N26 Si27 C28 111.85(14) . . ?
C29 Si27 C28 109.2(2) . . ?
C30 Si27 C28 105.0(2) . . ?
N26 Si31 C34 113.63(13) . . ?
N26 Si31 C32 108.78(11) . . ?
C34 Si31 C32 105.8(2) . . ?
N26 Si31 C33 113.06(13) . . ?
C34 Si31 C33 106.7(2) . . ?
C32 Si31 C33 108.51(14) . . ?
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
Zn N26 1.892(2) . ?
Zn N1 1.953(2) . ?
Zn N3 1.969(2) . ?
C1 N1 1.331(3) . ?
C1 C2 1.400(3) . ?
C1 C4 1.510(3) . ?
N1 C6 1.441(3) . ?
C2 C3 1.401(3) . ?
C3 N3 1.327(3) . ?
C3 C5 1.511(3) . ?
N3 C18 1.421(3) . ?
C6 C7 1.399(3) . ?
C6 C11 1.411(3) . ?
C7 C8 1.398(3) . ?
C7 C12 1.517(3) . ?
C8 C9 1.373(4) . ?
C9 C10 1.379(4) . ?
C10 C11 1.386(4) . ?
C11 C15 1.522(4) . ?
C12 C13 1.526(4) . ?
C12 C14 1.534(4) . ?
C15 C17 1.503(5) . ?
C15 C16 1.521(4) . ?
C18 C23 1.391(4) . ?
C18 C19 1.400(4) . ?
C19 O24 1.372(3) . ?
C19 C20 1.386(4) . ?
C20 C21 1.380(4) . ?
C21 C22 1.374(4) . ?
C22 C23 1.385(4) . ?
O24 C25 1.436(3) . ?
N26 Si27 1.709(2) . ?
N26 Si31 1.713(2) . ?
Si27 C29 1.870(3) . ?
Si27 C30 1.872(3) . ?
Si27 C28 1.873(3) . ?
Si31 C34 1.864(3) . ?
Si31 C32 1.868(3) . ?
Si31 C33 1.872(3) . ?
