#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:16:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180032 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/26/7032627.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_7032627
loop_
_publ_author_name
'Honrado, Manuel'
'Otero, Antonio'
'Fernández-Baeza, Juan'
'Sánchez-Barba, Luis F'
'Garcés, Andrés'
'Lara-Sánchez, Agustín'
'Rodríguez, Ana M'
_publ_section_title
;
 Enantiopure N,N,O-scorpionate zinc amide and chloride complexes as
 efficient initiators for the heteroselective ROP of cyclic esters.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17090
_journal_page_last               17100
_journal_paper_doi               10.1039/c4dt02178a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C25 H41 N5 O Si2 Zn'
_chemical_formula_sum            'C25 H41 N5 O Si2 Zn'
_chemical_formula_weight         549.18
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 124.508(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.746(9)
_cell_length_b                   10.760(4)
_cell_length_c                   21.751(8)
_cell_measurement_reflns_used    845
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      2.27
_cell_volume                     6123(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'WINGX v2013.3 (Farrugia)'
_computing_publication_material  'WINGX v2013.3 (Farrugia)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.1488
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16774
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.384
_diffrn_reflns_theta_min         3.115
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.861
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         9022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.1720
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0736P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3680
_reflns_number_total             9022
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt02178a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7032626--7032628.cif.'
_cod_database_code               7032627
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.819
_shelx_estimated_absorpt_t_max   0.876
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Zn1 Zn 0.16740(2) 0.10325(4) 0.57473(2) 0.04872(17) Uani 1 1 d . .
N1 N 0.15874(11) 0.1547(3) 0.65911(16) 0.0487(8) Uani 1 1 d . .
N2 N 0.20472(11) 0.1707(3) 0.72645(16) 0.0449(7) Uani 1 1 d . .
N3 N 0.22194(11) 0.2468(3) 0.61156(15) 0.0469(7) Uani 1 1 d . .
N4 N 0.25802(11) 0.2407(3) 0.68704(15) 0.0408(7) Uani 1 1 d . .
N5 N 0.11194(12) 0.0756(3) 0.47399(17) 0.0580(9) Uani 1 1 d . .
O4 O 0.21956(9) -0.0168(3) 0.63861(13) 0.0538(7) Uani 1 1 d . .
Si1 Si 0.10876(5) -0.07317(13) 0.44536(6) 0.0627(4) Uani 1 1 d . .
Si2 Si 0.07118(5) 0.19578(14) 0.42378(7) 0.0684(4) Uani 1 1 d . .
C1 C 0.19857(16) 0.1795(4) 0.7831(2) 0.0487(9) Uani 1 1 d . .
C2 C 0.14742(17) 0.1698(4) 0.7512(2) 0.0572(10) Uani 1 1 d . .
H2 H 0.1313 0.1729 0.7760 0.069 Uiso 1 1 calc R U
C3 C 0.12358(15) 0.1544(4) 0.6747(2) 0.0532(10) Uani 1 1 d . .
C4 C 0.24288(17) 0.1957(4) 0.8624(2) 0.0604(11) Uani 1 1 d . .
H4A H 0.2659 0.1267 0.8770 0.091 Uiso 1 1 calc R U
H4B H 0.2308 0.1995 0.8940 0.091 Uiso 1 1 calc R U
H4C H 0.2605 0.2714 0.8671 0.091 Uiso 1 1 calc R U
C5 C 0.06844(16) 0.1385(5) 0.6142(3) 0.0767(14) Uani 1 1 d . .
H5A H 0.0514 0.2172 0.6033 0.115 Uiso 1 1 calc R U
H5B H 0.0534 0.0807 0.6301 0.115 Uiso 1 1 calc R U
H5C H 0.0650 0.1072 0.5703 0.115 Uiso 1 1 calc R U
C6 C 0.29913(14) 0.3124(4) 0.7081(2) 0.0459(9) Uani 1 1 d . .
C7 C 0.28879(15) 0.3681(4) 0.6445(2) 0.0520(10) Uani 1 1 d . .
H7 H 0.3098 0.4232 0.6408 0.062 Uiso 1 1 calc R U
C8 C 0.24086(15) 0.3266(4) 0.5863(2) 0.0512(10) Uani 1 1 d . .
C9 C 0.34479(15) 0.3232(4) 0.7869(2) 0.0599(11) Uani 1 1 d . .
H9A H 0.3342 0.3509 0.8181 0.090 Uiso 1 1 calc R U
H9B H 0.3684 0.3821 0.7893 0.090 Uiso 1 1 calc R U
H9C H 0.3611 0.2437 0.8039 0.090 Uiso 1 1 calc R U
C10 C 0.21176(19) 0.3612(5) 0.5054(2) 0.0758(14) Uani 1 1 d . .
H10A H 0.1887 0.2952 0.4757 0.114 Uiso 1 1 calc R U
H10B H 0.2353 0.3745 0.4915 0.114 Uiso 1 1 calc R U
H10C H 0.1927 0.4360 0.4970 0.114 Uiso 1 1 calc R U
C11 C 0.25204(13) 0.1508(4) 0.73154(19) 0.0431(8) Uani 1 1 d . .
H11 H 0.2803 0.1640 0.7837 0.052 Uiso 1 1 calc R U
C12 C 0.25595(13) 0.0142(4) 0.71154(19) 0.0445(8) Uani 1 1 d . .
H12 H 0.2507 -0.0400 0.7429 0.053 Uiso 1 1 calc R U
C13 C 0.31075(13) -0.0046(3) 0.7353(2) 0.0446(8) Uani 1 1 d . .
C14 C 0.35017(15) -0.0194(4) 0.8093(2) 0.0541(10) Uani 1 1 d . .
H14 H 0.3430 -0.0211 0.8452 0.065 Uiso 1 1 calc R U
C15 C 0.39993(16) -0.0317(4) 0.8308(3) 0.0673(12) Uani 1 1 d . .
H15 H 0.4259 -0.0392 0.8813 0.081 Uiso 1 1 calc R U
C16 C 0.41223(17) -0.0331(5) 0.7792(3) 0.0724(13) Uani 1 1 d . .
C17 C 0.37237(19) -0.0190(5) 0.7046(3) 0.0740(13) Uani 1 1 d . .
H17 H 0.3795 -0.0186 0.6686 0.089 Uiso 1 1 calc R U
C18 C 0.32264(16) -0.0057(4) 0.6828(2) 0.0600(11) Uani 1 1 d . .
H18 H 0.2967 0.0026 0.6324 0.072 Uiso 1 1 calc R U
C19 C 0.46676(18) -0.0511(7) 0.8029(4) 0.108(2) Uani 1 1 d . .
H19A H 0.4679 -0.1160 0.7735 0.162 Uiso 1 1 calc R U
H19B H 0.4878 -0.0737 0.8547 0.162 Uiso 1 1 calc R U
H19C H 0.4792 0.0248 0.7955 0.162 Uiso 1 1 calc R U
C20 C 0.1708(2) -0.1221(5) 0.4615(3) 0.0826(15) Uani 1 1 d . .
H20A H 0.1777 -0.0719 0.4317 0.124 Uiso 1 1 calc R U
H20B H 0.1688 -0.2079 0.4478 0.124 Uiso 1 1 calc R U
H20C H 0.1979 -0.1118 0.5133 0.124 Uiso 1 1 calc R U
C21 C 0.0952(3) -0.1841(6) 0.4979(3) 0.106(2) Uani 1 1 d . .
H21A H 0.1220 -0.1792 0.5501 0.159 Uiso 1 1 calc R U
H21B H 0.0935 -0.2671 0.4804 0.159 Uiso 1 1 calc R U
H21C H 0.0631 -0.1632 0.4902 0.159 Uiso 1 1 calc R U
C22 C 0.0587(2) -0.1008(7) 0.3434(3) 0.122(3) Uani 1 1 d . .
H22A H 0.0254 -0.0852 0.3329 0.184 Uiso 1 1 calc R U
H22B H 0.0605 -0.1854 0.3311 0.184 Uiso 1 1 calc R U
H22C H 0.0644 -0.0459 0.3141 0.184 Uiso 1 1 calc R U
C23 C 0.00269(17) 0.1614(7) 0.3856(3) 0.0964(18) Uani 1 1 d . .
H23A H -0.0081 0.0889 0.3544 0.145 Uiso 1 1 calc R U
H23B H -0.0182 0.2309 0.3566 0.145 Uiso 1 1 calc R U
H23C H -0.0008 0.1467 0.4260 0.145 Uiso 1 1 calc R U
C24 C 0.0731(2) 0.2411(6) 0.3421(3) 0.0953(18) Uani 1 1 d . .
H24A H 0.1075 0.2628 0.3594 0.143 Uiso 1 1 calc R U
H24B H 0.0511 0.3111 0.3172 0.143 Uiso 1 1 calc R U
H24C H 0.0618 0.1725 0.3080 0.143 Uiso 1 1 calc R U
C25 C 0.08768(19) 0.3367(5) 0.4839(3) 0.0860(16) Uani 1 1 d . .
H25A H 0.0854 0.3170 0.5250 0.129 Uiso 1 1 calc R U
H25B H 0.0642 0.4025 0.4550 0.129 Uiso 1 1 calc R U
H25C H 0.1219 0.3626 0.5026 0.129 Uiso 1 1 calc R U
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'
Si Si 0.0817 0.0704 '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
N5 Zn1 O4 125.50(13)
N5 Zn1 N1 124.02(14)
O4 Zn1 N1 91.79(12)
N5 Zn1 N3 125.20(13)
O4 Zn1 N3 91.82(12)
N1 Zn1 N3 87.74(12)
C3 N1 N2 105.4(3)
C3 N1 Zn1 140.3(3)
N2 N1 Zn1 112.5(2)
C1 N2 N1 111.4(3)
C1 N2 C11 127.9(3)
N1 N2 C11 119.3(3)
C8 N3 N4 105.0(3)
C8 N3 Zn1 141.2(3)
N4 N3 Zn1 111.6(2)
C6 N4 N3 111.7(3)
C6 N4 C11 128.1(3)
N3 N4 C11 119.5(3)
Si1 N5 Si2 127.62(19)
Si1 N5 Zn1 113.16(18)
Si2 N5 Zn1 119.2(2)
C12 O4 Zn1 119.1(2)
N5 Si1 C21 111.4(2)
N5 Si1 C20 111.0(2)
C21 Si1 C20 106.8(3)
N5 Si1 C22 114.6(3)
C21 Si1 C22 106.7(3)
C20 Si1 C22 105.9(3)
N5 Si2 C25 110.74(19)
N5 Si2 C23 113.7(2)
C25 Si2 C23 105.4(3)
N5 Si2 C24 112.4(3)
C25 Si2 C24 107.8(3)
C23 Si2 C24 106.5(2)
N2 C1 C2 106.0(3)
N2 C1 C4 122.0(4)
C2 C1 C4 132.0(4)
C1 C2 C3 107.6(4)
N1 C3 C2 109.6(3)
N1 C3 C5 120.6(4)
C2 C3 C5 129.8(4)
N4 C6 C7 105.9(3)
N4 C6 C9 123.8(3)
C7 C6 C9 130.3(4)
C6 C7 C8 107.0(3)
N3 C8 C7 110.3(3)
N3 C8 C10 121.5(4)
C7 C8 C10 128.2(4)
N4 C11 N2 111.6(3)
N4 C11 C12 112.4(3)
N2 C11 C12 111.0(3)
O4 C12 C13 114.3(3)
O4 C12 C11 113.8(3)
C13 C12 C11 106.7(3)
C14 C13 C18 117.9(4)
C14 C13 C12 121.3(3)
C18 C13 C12 120.8(3)
C15 C14 C13 121.1(4)
C14 C15 C16 121.5(4)
C15 C16 C17 117.3(4)
C15 C16 C19 121.3(5)
C17 C16 C19 121.4(5)
C18 C17 C16 121.5(4)
C17 C18 C13 120.7(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Zn1 N5 1.902(3)
Zn1 O4 1.932(3)
Zn1 N1 2.079(3)
Zn1 N3 2.111(3)
N1 C3 1.338(5)
N1 N2 1.372(4)
N2 C1 1.356(4)
N2 C11 1.458(5)
N3 C8 1.332(5)
N3 N4 1.372(4)
N4 C6 1.352(4)
N4 C11 1.455(5)
N5 Si1 1.700(4)
N5 Si2 1.714(4)
O4 C12 1.373(4)
Si1 C21 1.863(6)
Si1 C20 1.871(5)
Si1 C22 1.882(5)
Si2 C25 1.873(6)
Si2 C23 1.873(5)
Si2 C24 1.876(5)
C1 C2 1.361(6)
C1 C4 1.495(5)
C2 C3 1.394(5)
C3 C5 1.488(6)
C6 C7 1.367(5)
C6 C9 1.495(5)
C7 C8 1.391(5)
C8 C10 1.499(5)
C11 C12 1.558(5)
C12 C13 1.522(5)
C13 C14 1.378(5)
C13 C18 1.391(5)
C14 C15 1.376(6)
C15 C16 1.383(7)
C16 C17 1.390(7)
C16 C19 1.513(7)
C17 C18 1.375(6)
