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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/4/07/12/4071267.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_4071267
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            'C20 H40 Br2 N2 O4 Zn2'
_chemical_formula_weight         663.10
_chemical_name_common            '{BrZn[CH2C(O)NEt2](thf)}2, (1a)'
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.5370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6870(5)
_cell_length_b                   8.8254(4)
_cell_length_c                   14.8247(7)
_cell_measurement_temperature    151(2)
_cell_volume                     1378.90(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      151(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0783
_diffrn_reflns_av_sigmaI/netI    0.1018
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10751
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    4.662
_exptl_absorpt_correction_T_max  0.6528
_exptl_absorpt_correction_T_min  0.4557
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0476
_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)+(0.0260P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                2383
_reflns_number_total             3280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800070j-file001.cif
_cod_data_source_block           jrh083
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4071267
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.89624(4) 0.83763(4) 0.01297(3) 0.02189(15) Uani 1 1 d .
Br2 Br 0.93769(4) 0.74745(5) 0.16544(3) 0.03409(15) Uani 1 1 d .
O1 O 1.0352(3) 0.7772(3) -0.05394(19) 0.0234(6) Uani 1 1 d .
O2 O 0.7746(3) 0.6803(3) -0.05973(19) 0.0257(6) Uani 1 1 d .
N1 N 1.2147(3) 0.8133(3) -0.1098(2) 0.0246(8) Uani 1 1 d .
C1 C 0.8215(4) 1.0444(4) -0.0250(3) 0.0221(8) Uani 1 1 d .
H1A H 0.8513 1.0778 -0.0816 0.031 Uiso 1 1 calc R
H1B H 0.7278 1.0373 -0.0379 0.031 Uiso 1 1 calc R
C2 C 1.1405(4) 0.8456(4) -0.0471(3) 0.0211(8) Uani 1 1 d .
C3 C 1.1699(5) 0.7083(4) -0.1847(3) 0.0294(10) Uani 1 1 d .
H3A H 1.1179 0.6283 -0.1621 0.041 Uiso 1 1 calc R
H3B H 1.2439 0.6588 -0.2044 0.041 Uiso 1 1 calc R
C4 C 1.0914(5) 0.7862(6) -0.2664(3) 0.0432(12) Uani 1 1 d .
H4A H 1.0640 0.7114 -0.3144 0.065 Uiso 1 1 calc R
H4B H 1.1429 0.8642 -0.2898 0.065 Uiso 1 1 calc R
H4C H 1.0168 0.8334 -0.2476 0.065 Uiso 1 1 calc R
C5 C 1.3352(4) 0.8902(5) -0.1127(3) 0.0316(10) Uani 1 1 d .
H5A H 1.3321 0.9931 -0.0866 0.044 Uiso 1 1 calc R
H5B H 1.3469 0.9013 -0.1773 0.044 Uiso 1 1 calc R
C6 C 1.4468(5) 0.8062(6) -0.0609(4) 0.0482(13) Uani 1 1 d .
H6A H 1.5250 0.8618 -0.0651 0.072 Uiso 1 1 calc R
H6B H 1.4512 0.7049 -0.0872 0.072 Uiso 1 1 calc R
H6C H 1.4369 0.7973 0.0035 0.072 Uiso 1 1 calc R
C7 C 0.7523(5) 0.6978(4) -0.1583(3) 0.0306(10) Uani 1 1 d .
H7A H 0.8198 0.7604 -0.1780 0.043 Uiso 1 1 calc R
H7B H 0.6694 0.7472 -0.1791 0.043 Uiso 1 1 calc R
C8 C 0.7533(6) 0.5407(5) -0.1974(4) 0.0523(15) Uani 1 1 d .
H8A H 0.6879 0.5299 -0.2526 0.073 Uiso 1 1 calc R
H8B H 0.8374 0.5161 -0.2133 0.073 Uiso 1 1 calc R
C9 C 0.7243(6) 0.4413(5) -0.1216(4) 0.0548(16) Uani 1 1 d .
H9A H 0.6317 0.4337 -0.1225 0.077 Uiso 1 1 calc R
H9B H 0.7594 0.3382 -0.1261 0.077 Uiso 1 1 calc R
C10 C 0.7881(6) 0.5200(4) -0.0370(4) 0.0507(15) Uani 1 1 d .
H10A H 0.7461 0.4952 0.0158 0.071 Uiso 1 1 calc R
H10B H 0.8787 0.4910 -0.0224 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'
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 C1 113.18(14) . .
O1 Zn1 O2 90.95(11) . .
C1 Zn1 O2 105.84(14) . .
O1 Zn1 Br2 110.39(9) . .
C1 Zn1 Br2 124.66(11) . .
O2 Zn1 Br2 105.82(8) . .
O1 Zn1 Zn1 69.18(7) . 3_775
C1 Zn1 Zn1 59.23(12) . 3_775
O2 Zn1 Zn1 143.30(8) . 3_775
Br2 Zn1 Zn1 109.92(2) . 3_775
C2 O1 Zn1 123.9(2) . .
C7 O2 C10 109.3(3) . .
C7 O2 Zn1 115.9(2) . .
C10 O2 Zn1 120.0(3) . .
C2 N1 C5 122.9(3) . .
C2 N1 C3 120.0(4) . .
C5 N1 C3 116.8(3) . .
C2 C1 Zn1 110.3(3) 3_775 .
O1 C2 N1 117.4(3) . .
O1 C2 C1 121.0(3) . 3_775
N1 C2 C1 121.6(4) . 3_775
N1 C3 C4 112.7(4) . .
N1 C5 C6 112.6(4) . .
O2 C7 C8 106.3(3) . .
C9 C8 C7 103.6(4) . .
C10 C9 C8 103.5(4) . .
O2 C10 C9 104.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.991(3) .
Zn1 C1 2.034(4) .
Zn1 O2 2.077(3) .
Zn1 Br2 2.3678(6) .
Zn1 Zn1 3.6828(8) 3_775
O1 C2 1.266(5) .
O2 C7 1.449(5) .
O2 C10 1.456(5) .
N1 C2 1.349(5) .
N1 C5 1.463(5) .
N1 C3 1.464(5) .
C1 C2 1.451(5) 3_775
C2 C1 1.451(5) 3_775
C3 C4 1.518(7) .
C5 C6 1.503(7) .
C7 C8 1.503(6) .
C8 C9 1.498(7) .
C9 C10 1.495(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
C1 Zn1 O1 C2 65.0(3) . .
O2 Zn1 O1 C2 172.7(3) . .
Br2 Zn1 O1 C2 -80.1(3) . .
Zn1 Zn1 O1 C2 24.3(3) 3_775 .
O1 Zn1 O2 C7 -58.5(3) . .
C1 Zn1 O2 C7 55.9(3) . .
Br2 Zn1 O2 C7 -170.1(2) . .
Zn1 Zn1 O2 C7 -3.5(3) 3_775 .
O1 Zn1 O2 C10 76.2(3) . .
C1 Zn1 O2 C10 -169.4(3) . .
Br2 Zn1 O2 C10 -35.4(3) . .
Zn1 Zn1 O2 C10 131.2(3) 3_775 .
O1 Zn1 C1 C2 -108.2(3) . 3_775
O2 Zn1 C1 C2 153.8(3) . 3_775
Br2 Zn1 C1 C2 31.0(3) . 3_775
Zn1 Zn1 C1 C2 -63.0(3) 3_775 3_775
Zn1 O1 C2 N1 -166.3(3) . .
Zn1 O1 C2 C1 12.9(5) . 3_775
C5 N1 C2 O1 176.6(4) . .
C3 N1 C2 O1 2.9(5) . .
C5 N1 C2 C1 -2.7(6) . 3_775
C3 N1 C2 C1 -176.4(4) . 3_775
C2 N1 C3 C4 86.5(5) . .
C5 N1 C3 C4 -87.6(5) . .
C2 N1 C5 C6 93.7(5) . .
C3 N1 C5 C6 -92.4(5) . .
C10 O2 C7 C8 -0.5(5) . .
Zn1 O2 C7 C8 138.9(3) . .
O2 C7 C8 C9 22.1(6) . .
C7 C8 C9 C10 -34.8(6) . .
C7 O2 C10 C9 -21.4(6) . .
Zn1 O2 C10 C9 -158.8(4) . .
C8 C9 C10 O2 34.7(6) . .
