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#$Date: 2016-03-21 08:17:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178601 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/12/4071268.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_4071268
loop_
_publ_author_name
'Greco, Jeffrey F.'
'McNevin, Michael J.'
'Shoemaker, Richard K.'
'Hagadorn, John R.'
_publ_section_title
;
 Solid- and Solution-Phase Structures of Zinc Enolates of Amides and
 Ketones
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1948
_journal_paper_doi               10.1021/om800070j
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C16 H36 Br2 N2 O4 S2 Zn2'
_chemical_formula_weight         675.15
_chemical_name_common            '{BrZn[CH2C(O)NEt2](dmso)}2, (1b)'
_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                103.4460(10)
_cell_angle_beta                 99.1770(10)
_cell_angle_gamma                106.3370(10)
_cell_formula_units_Z            1
_cell_length_a                   8.0442(4)
_cell_length_b                   9.6895(5)
_cell_length_c                   9.9379(5)
_cell_measurement_temperature    147(2)
_cell_volume                     701.65(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5389
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    4.726
_exptl_absorpt_correction_T_max  0.3314
_exptl_absorpt_correction_T_min  0.2010
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.119
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         3269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0512
_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)+(0.0936P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                2787
_reflns_number_total             3269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800070j-file001.cif
_cod_data_source_block           jrh086
_cod_original_sg_symbol_H-M      'P-1 (#2)'
_cod_database_code               4071268
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
Zn1 Zn 0.38117(5) -0.17356(4) 0.54228(4) 0.02358(15) Uani 1 1 d .
S1 S 0.25539(11) -0.51510(9) 0.42362(10) 0.0283(2) Uani 1 1 d .
O1 O 0.4773(3) -0.2171(3) 0.3711(2) 0.0257(5) Uani 1 1 d .
O2 O 0.1944(3) -0.3804(3) 0.4793(3) 0.0336(6) Uani 1 1 d .
N1 N 0.6191(4) -0.1673(3) 0.2031(3) 0.0277(6) Uani 1 1 d .
Br1 Br 0.57909(5) -0.18457(5) 0.74491(4) 0.03761(16) Uani 1 1 d .
C1 C 0.2709(4) -0.0082(4) 0.5553(3) 0.0240(6) Uani 1 1 d .
H1A H 0.2463 0.0099 0.4612 0.034 Uiso 1 1 calc R
H1B H 0.1565 -0.0387 0.5835 0.034 Uiso 1 1 calc R
C2 C 0.6057(4) -0.1293(4) 0.3391(3) 0.0223(6) Uani 1 1 d .
C3 C 0.4882(5) -0.3037(5) 0.1008(4) 0.0365(8) Uani 1 1 d .
H3A H 0.4619 -0.3840 0.1481 0.051 Uiso 1 1 calc R
H3B H 0.5410 -0.3377 0.0211 0.051 Uiso 1 1 calc R
C4 C 0.3155(6) -0.2821(6) 0.0411(5) 0.0551(12) Uani 1 1 d .
H4A H 0.2616 -0.2495 0.1192 0.083 Uiso 1 1 calc R
H4B H 0.2331 -0.3773 -0.0255 0.083 Uiso 1 1 calc R
H4C H 0.3397 -0.2054 -0.0091 0.083 Uiso 1 1 calc R
C5 C 0.7547(6) -0.0747(5) 0.1492(4) 0.0403(9) Uani 1 1 d .
H5A H 0.7923 0.0313 0.2083 0.056 Uiso 1 1 calc R
H5B H 0.7019 -0.0798 0.0504 0.056 Uiso 1 1 calc R
C6 C 0.9168(6) -0.1248(7) 0.1508(6) 0.0610(14) Uani 1 1 d .
H6A H 0.9755 -0.1120 0.2494 0.091 Uiso 1 1 calc R
H6B H 1.0003 -0.0639 0.1084 0.091 Uiso 1 1 calc R
H6C H 0.8797 -0.2310 0.0958 0.091 Uiso 1 1 calc R
C7 C 0.2169(6) -0.6232(5) 0.5446(5) 0.0425(10) Uani 1 1 d .
H7A H 0.3037 -0.5701 0.6364 0.064 Uiso 1 1 calc R
H7B H 0.2299 -0.7212 0.5059 0.064 Uiso 1 1 calc R
H7C H 0.0958 -0.6379 0.5583 0.064 Uiso 1 1 calc R
C8 C 0.0744(6) -0.6319(5) 0.2748(5) 0.0475(10) Uani 1 1 d .
H8A H -0.0378 -0.6504 0.3053 0.071 Uiso 1 1 calc R
H8B H 0.0929 -0.7279 0.2373 0.071 Uiso 1 1 calc R
H8C H 0.0689 -0.5814 0.2003 0.071 Uiso 1 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 0.0033 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'
S S 0.1246 0.1234 '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'
Br Br -0.2901 2.4595 '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
O1 Zn1 O2 92.56(10) . .
O1 Zn1 C1 114.13(12) . .
O2 Zn1 C1 112.16(12) . .
O1 Zn1 Br1 109.59(7) . .
O2 Zn1 Br1 102.14(8) . .
C1 Zn1 Br1 121.73(9) . .
O1 Zn1 Zn1 67.28(7) . 2_656
O2 Zn1 Zn1 149.64(8) . 2_656
C1 Zn1 Zn1 61.40(10) . 2_656
Br1 Zn1 Zn1 105.898(19) . 2_656
O2 S1 C7 104.61(19) . .
O2 S1 C8 102.51(18) . .
C7 S1 C8 99.2(2) . .
C2 O1 Zn1 127.5(2) . .
S1 O2 Zn1 117.15(14) . .
C2 N1 C3 119.4(3) . .
C2 N1 C5 123.1(3) . .
C3 N1 C5 117.3(3) . .
C2 C1 Zn1 109.1(2) 2_656 .
O1 C2 N1 116.9(3) . .
O1 C2 C1 121.3(3) . 2_656
N1 C2 C1 121.8(3) . 2_656
N1 C3 C4 113.4(4) . .
N1 C5 C6 112.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.985(2) .
Zn1 O2 2.022(3) .
Zn1 C1 2.028(3) .
Zn1 Br1 2.4030(5) .
Zn1 Zn1 3.7260(7) 2_656
S1 O2 1.537(3) .
S1 C7 1.778(4) .
S1 C8 1.787(4) .
O1 C2 1.276(4) .
N1 C2 1.346(4) .
N1 C3 1.463(5) .
N1 C5 1.463(5) .
C1 C2 1.461(4) 2_656
C2 C1 1.461(4) 2_656
C3 C4 1.512(6) .
C5 C6 1.514(7) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 Zn1 O1 C2 179.6(3) . .
C1 Zn1 O1 C2 63.9(3) . .
Br1 Zn1 O1 C2 -76.5(3) . .
Zn1 Zn1 O1 C2 23.0(2) 2_656 .
C7 S1 O2 Zn1 117.9(2) . .
C8 S1 O2 Zn1 -139.0(2) . .
O1 Zn1 O2 S1 45.33(18) . .
C1 Zn1 O2 S1 162.72(17) . .
Br1 Zn1 O2 S1 -65.34(18) . .
Zn1 Zn1 O2 S1 91.8(2) 2_656 .
O1 Zn1 C1 C2 -103.7(2) . 2_656
O2 Zn1 C1 C2 152.7(2) . 2_656
Br1 Zn1 C1 C2 31.4(3) . 2_656
Zn1 Zn1 C1 C2 -60.3(2) 2_656 2_656
Zn1 O1 C2 N1 -163.6(2) . .
Zn1 O1 C2 C1 14.7(4) . 2_656
C3 N1 C2 O1 0.4(5) . .
C5 N1 C2 O1 177.4(3) . .
C3 N1 C2 C1 -178.0(3) . 2_656
C5 N1 C2 C1 -0.9(5) . 2_656
C2 N1 C3 C4 81.3(4) . .
C5 N1 C3 C4 -95.9(4) . .
C2 N1 C5 C6 95.6(4) . .
C3 N1 C5 C6 -87.3(4) . .
