#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/27/4112701.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_4112701
loop_
_publ_author_name
'Tomoaki Hamada'
'Kei Manabe'
'Shū Kobayashi'
_publ_section_title
;
 Enantio- and Diastereoselective, Stereospecific Mannich-Type Reactions in
 Water
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7768
_journal_page_last               7769
_journal_paper_doi               10.1021/ja048607t
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C31 H32 Cl4 N2 O2 Zn'
_chemical_formula_weight         671.80
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      96
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_audit_creation_date             'Fri Jan 30 21:52:28 2004'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4952(4)
_cell_length_b                   11.4952(4)
_cell_length_c                   47.840(2)
_cell_measurement_reflns_used    22173
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.8
_cell_volume                     6321.6(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_measured_fraction_theta_full 0.9140
_diffrn_measured_fraction_theta_max 0.9140
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15392
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  0.400
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_size_max          1.600
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          0.800
_refine_diff_density_max         1.84
_refine_diff_density_min         -1.47
_refine_ls_abs_structure_Flack   0.38(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.012
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     362
_refine_ls_number_reflns         3885
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.9420
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.06000(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                2404
_reflns_number_total             3889
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja048607tsi20040309_092803.cif
_cod_data_source_block           031010TH
_cod_original_sg_symbol_H-M      'P 43 21 2 '
_cod_original_formula_sum        'C31 H32 Cl4 N2 O2 Zn '
_cod_database_code               4112701
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,1/2+z
1/2-y,1/2+x,3/4+z
1/2+y,1/2-x,1/4+z
y,x,-z
-y,-x,1/2-z
1/2-x,1/2+y,3/4-z
1/2+x,1/2-y,1/4-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_calc_flag
Zn(1) Zn -0.26781(7) -0.11270(8) -0.14490(2) 0.0260(2) Uani 1.00 d
Cl(1) Cl -0.3853(2) 0.0322(2) -0.15352(4) 0.0324(5) Uani 1.00 d
Cl(2) Cl -0.3322(2) -0.2931(2) -0.15428(5) 0.0370(5) Uani 1.00 d
Cl(3) Cl -0.5515(2) 0.0054(2) -0.21804(5) 0.0492(7) Uani 1.00 d
Cl(4) Cl -0.5597(2) -0.2381(2) -0.23241(6) 0.0525(7) Uani 1.00 d
O(1) O -0.2367(5) -0.0126(5) -0.0461(1) 0.039(2) Uani 1.00 d
O(2) O 0.037(1) -0.157(1) -0.2137(3) 0.151(5) Uani 1.00 d
N(1) N -0.1886(5) -0.1120(6) -0.1062(1) 0.030(1) Uani 1.00 d
N(2) N -0.1004(5) -0.0938(5) -0.1618(1) 0.026(1) Uani 1.00 d
C(1) C -0.2224(9) 0.0781(10) -0.0267(2) 0.063(3) Uani 1.00 d
C(2) C -0.3489(6) -0.0337(8) -0.0555(2) 0.031(2) Uani 1.00 d
C(3) C -0.4465(7) 0.0244(8) -0.0466(2) 0.036(2) Uani 1.00 d
C(4) C -0.5557(7) -0.0065(9) -0.0570(2) 0.039(2) Uani 1.00 d
C(5) C -0.5627(7) -0.0932(8) -0.0770(2) 0.037(2) Uani 1.00 d
C(6) C -0.4648(7) -0.1498(9) -0.0855(2) 0.040(2) Uani 1.00 d
C(7) C -0.3565(6) -0.1258(7) -0.0752(2) 0.026(2) Uani 1.00 d
C(8) C -0.2520(7) -0.1864(7) -0.0854(2) 0.032(2) Uani 1.00 d
C(9) C -0.0660(6) -0.1513(6) -0.1120(2) 0.025(2) Uani 1.00 d
C(10) C 0.0125(6) -0.1433(6) -0.0877(2) 0.025(2) Uani 1.00 d
C(11) C 0.0307(7) -0.0404(7) -0.0726(2) 0.030(2) Uani 1.00 d
C(12) C 0.1072(7) -0.0329(8) -0.0504(2) 0.034(2) Uani 1.00 d
C(13) C 0.1707(7) -0.1311(7) -0.0423(2) 0.032(2) Uani 1.00 d
C(14) C 0.1547(7) -0.2325(7) -0.0564(2) 0.036(2) Uani 1.00 d
C(15) C 0.0766(7) -0.2428(7) -0.0790(2) 0.034(2) Uani 1.00 d
C(16) C 0.1990(7) -0.0455(8) -0.1429(2) 0.034(2) Uani 1.00 d
C(17) C 0.3109(8) -0.088(1) -0.1468(2) 0.054(2) Uani 1.00 d
C(18) C 0.3282(8) -0.2038(10) -0.1536(2) 0.051(2) Uani 1.00 d
C(19) C 0.2359(8) -0.2769(9) -0.1568(2) 0.048(2) Uani 1.00 d
C(20) C 0.1258(7) -0.2377(7) -0.1524(2) 0.037(2) Uani 1.00 d
C(21) C 0.1040(6) -0.1216(7) -0.1446(2) 0.023(1) Uani 1.00 d
C(22) C -0.0181(6) -0.0820(6) -0.1372(2) 0.025(2) Uani 1.00 d
C(23) C -0.0828(7) 0.0035(6) -0.1822(2) 0.030(2) Uani 1.00 d
C(24) C -0.1248(7) -0.0272(8) -0.2111(2) 0.037(2) Uani 1.00 d
C(25) C -0.2136(10) 0.0338(10) -0.2254(3) 0.074(4) Uani 1.00 d
C(26) C -0.247(1) 0.0059(9) -0.2528(3) 0.079(4) Uani 1.00 d
C(27) C -0.1917(8) -0.0827(9) -0.2652(2) 0.052(3) Uani 1.00 d
C(28) C -0.1025(9) -0.141(1) -0.2528(2) 0.061(3) Uani 1.00 d
C(29) C -0.067(1) -0.113(1) -0.2254(2) 0.067(3) Uani 1.00 d
C(30) C 0.137(2) -0.235(4) -0.2271(7) 0.34(2) Uani 1.00 d
C(31) C -0.4839(8) -0.1274(8) -0.2147(2) 0.039(2) Uani 1.00 d
H(1) H -0.1432 0.0843 -0.0216 0.0774 Uiso 1.00 calc
H(2) H -0.2681 0.0624 -0.0105 0.0774 Uiso 1.00 calc
H(3) H -0.2478 0.1492 -0.0349 0.0774 Uiso 1.00 calc
H(4) H -0.4395 0.0853 -0.0331 0.0420 Uiso 1.00 calc
H(5) H -0.6232 0.0327 -0.0508 0.0468 Uiso 1.00 calc
H(6) H -0.6357 -0.1135 -0.0847 0.0442 Uiso 1.00 calc
H(7) H -0.4720 -0.2063 -0.0997 0.0481 Uiso 1.00 calc
H(8) H -0.2734 -0.2575 -0.0938 0.0374 Uiso 1.00 calc
H(9) H -0.2015 -0.2021 -0.0698 0.0374 Uiso 1.00 calc
H(10) H -0.1860 -0.0344 -0.0993 0.0357 Uiso 1.00 calc
H(11) H -0.0117 0.0270 -0.0779 0.0358 Uiso 1.00 calc
H(12) H 0.1156 0.0389 -0.0407 0.0400 Uiso 1.00 calc
H(13) H 0.2239 -0.1265 -0.0272 0.0385 Uiso 1.00 calc
H(14) H 0.1971 -0.2994 -0.0509 0.0441 Uiso 1.00 calc
H(15) H 0.0667 -0.3152 -0.0883 0.0406 Uiso 1.00 calc
H(16) H -0.0695 -0.2310 -0.1174 0.0295 Uiso 1.00 calc
H(17) H 0.1870 0.0340 -0.1389 0.0406 Uiso 1.00 calc
H(18) H 0.3763 -0.0373 -0.1451 0.0642 Uiso 1.00 calc
H(19) H 0.4044 -0.2323 -0.1561 0.0614 Uiso 1.00 calc
H(20) H 0.2476 -0.3556 -0.1621 0.0572 Uiso 1.00 calc
H(21) H 0.0622 -0.2896 -0.1548 0.0441 Uiso 1.00 calc
H(22) H -0.0145 -0.0025 -0.1320 0.0302 Uiso 1.00 calc
H(23) H -0.0815 -0.1641 -0.1712 0.0307 Uiso 1.00 calc
H(24) H -0.1250 0.0695 -0.1758 0.0366 Uiso 1.00 calc
H(25) H -0.0025 0.0216 -0.1830 0.0366 Uiso 1.00 calc
H(26) H -0.2521 0.0960 -0.2160 0.0862 Uiso 1.00 calc
H(27) H -0.3051 0.0482 -0.2622 0.0923 Uiso 1.00 calc
H(28) H -0.2153 -0.1059 -0.2833 0.0611 Uiso 1.00 calc
H(29) H -0.0632 -0.2000 -0.2627 0.0754 Uiso 1.00 calc
H(30) H 0.1119 -0.3091 -0.2360 0.2779 Uiso 1.00 calc
H(31) H 0.1759 -0.1957 -0.2445 0.2779 Uiso 1.00 calc
H(32) H 0.2034 -0.2546 -0.2161 0.2779 Uiso 1.00 calc
H(33) H -0.4076 -0.1216 -0.2221 0.0461 Uiso 1.00 calc
H(34) H -0.4798 -0.1466 -0.1954 0.0461 Uiso 1.00 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Zn Zn 0.284 1.430
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
