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#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075491.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_4075491
loop_
_publ_author_name
'Mountford, Andrew J.'
'Lancaster, Simon J.'
'Coles, Simon J.'
'Horton, Peter N.'
'Hughes, David L.'
'Hursthouse, Michael B.'
'Light, Mark E.'
_publ_section_title
;
 The Synthesis, Molecular Structures, and Supramolecular Architecture of
 Amine Adducts of Bis(pentafluorophenyl)zinc
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3837
_journal_paper_doi               10.1021/om060319d
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C30 H26 F10 N2 Zn'
_chemical_formula_weight         669.90
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 118.437(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.8942(6)
_cell_length_b                   8.7771(2)
_cell_length_c                   16.1559(3)
_cell_measurement_reflns_used    18332
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2854.73(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19251
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.7973
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0294
_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)+(0.0308P)²+3.0765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                3081
_reflns_number_total             3267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060319dsi20060602_044627.cif
_cod_data_source_block           comp8
_cod_original_cell_volume        2854.73(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4075491
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.46053(8) 0.80683(17) 0.81999(11) 0.0242(3) Uani 1 1 d .
C2 C 0.48215(8) 0.95337(18) 0.85189(11) 0.0249(3) Uani 1 1 d .
C3 C 0.45409(8) 1.04694(18) 0.89176(11) 0.0279(3) Uani 1 1 d .
C4 C 0.40203(9) 0.99313(19) 0.90375(12) 0.0292(3) Uani 1 1 d .
C5 C 0.37954(8) 0.8468(2) 0.87625(11) 0.0284(3) Uani 1 1 d .
C6 C 0.40911(8) 0.75970(18) 0.83569(11) 0.0265(3) Uani 1 1 d .
C7 C 0.45298(9) 0.5033(2) 0.57481(13) 0.0346(4) Uani 1 1 d .
H7A H 0.4946 0.4469 0.6096 0.052 Uiso 1 1 calc R
H7B H 0.4612 0.5958 0.5479 0.052 Uiso 1 1 calc R
H7C H 0.4205 0.4393 0.5241 0.052 Uiso 1 1 calc R
C8 C 0.40749(9) 0.40406(19) 0.67025(13) 0.0345(4) Uani 1 1 d .
H8A H 0.3727 0.3517 0.6153 0.052 Uiso 1 1 calc R
H8B H 0.3907 0.4293 0.7142 0.052 Uiso 1 1 calc R
H8C H 0.4463 0.3373 0.7015 0.052 Uiso 1 1 calc R
C9 C 0.36816(8) 0.65011(18) 0.59111(11) 0.0261(3) Uani 1 1 d .
H9A H 0.3827 0.7422 0.5706 0.031 Uiso 1 1 calc R
H9B H 0.3541 0.6830 0.6375 0.031 Uiso 1 1 calc R
C10 C 0.30850(8) 0.58424(17) 0.50672(11) 0.0264(3) Uani 1 1 d .
C11 C 0.30311(9) 0.5887(2) 0.41716(12) 0.0320(4) Uani 1 1 d .
H11 H 0.3374 0.6343 0.4084 0.038 Uiso 1 1 calc R
C12 C 0.24820(9) 0.5273(2) 0.34074(12) 0.0371(4) Uani 1 1 d .
H12 H 0.2453 0.5297 0.2801 0.045 Uiso 1 1 calc R
C13 C 0.19750(9) 0.4624(2) 0.35230(13) 0.0351(4) Uani 1 1 d .
H13 H 0.1599 0.4204 0.2998 0.042 Uiso 1 1 calc R
C14 C 0.20182(9) 0.4588(2) 0.44062(13) 0.0335(4) Uani 1 1 d .
H14 H 0.1670 0.4150 0.4489 0.040 Uiso 1 1 calc R
C15 C 0.25712(8) 0.51941(19) 0.51714(12) 0.0300(3) Uani 1 1 d .
H15 H 0.2599 0.5165 0.5777 0.036 Uiso 1 1 calc R
N1 N 0.42671(7) 0.54566(15) 0.63969(10) 0.0258(3) Uani 1 1 d .
F1 F 0.53457(5) 1.01261(11) 0.84570(7) 0.0320(2) Uani 1 1 d .
F2 F 0.47611(6) 1.18984(11) 0.91953(8) 0.0373(2) Uani 1 1 d .
F3 F 0.37378(6) 1.08195(12) 0.94224(8) 0.0412(3) Uani 1 1 d .
F4 F 0.32938(6) 0.79390(13) 0.88905(8) 0.0387(3) Uani 1 1 d .
F5 F 0.38410(5) 0.61626(11) 0.81009(7) 0.0344(2) Uani 1 1 d .
Zn1 Zn 0.5000 0.68675(3) 0.7500 0.02261(9) Uani 1 2 d S
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'
F F 0.0171 0.0103 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C6 C1 C2 113.23(15) . .
C6 C1 Zn1 125.98(11) . .
C2 C1 Zn1 120.68(12) . .
F1 C2 C3 115.64(14) . .
F1 C2 C1 120.04(14) . .
C3 C2 C1 124.31(15) . .
F2 C3 C2 121.83(16) . .
F2 C3 C4 118.93(15) . .
C2 C3 C4 119.24(15) . .
F3 C4 C5 120.23(16) . .
F3 C4 C3 120.43(15) . .
C5 C4 C3 119.34(15) . .
F4 C5 C4 119.27(15) . .
F4 C5 C6 122.13(15) . .
C4 C5 C6 118.59(15) . .
F5 C6 C5 115.25(14) . .
F5 C6 C1 119.52(14) . .
C5 C6 C1 125.24(15) . .
N1 C7 H7A 109.5 . .
N1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N1 C8 H8A 109.5 . .
N1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N1 C9 C10 115.88(13) . .
N1 C9 H9A 108.3 . .
C10 C9 H9A 108.3 . .
N1 C9 H9B 108.3 . .
C10 C9 H9B 108.3 . .
H9A C9 H9B 107.4 . .
C15 C10 C11 118.47(15) . .
C15 C10 C9 120.11(15) . .
C11 C10 C9 121.42(15) . .
C12 C11 C10 120.60(16) . .
C12 C11 H11 119.7 . .
C10 C11 H11 119.7 . .
C13 C12 C11 120.26(17) . .
C13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
C14 C13 C12 119.76(16) . .
C14 C13 H13 120.1 . .
C12 C13 H13 120.1 . .
C13 C14 C15 119.83(17) . .
C13 C14 H14 120.1 . .
C15 C14 H14 120.1 . .
C14 C15 C10 121.06(16) . .
C14 C15 H15 119.5 . .
C10 C15 H15 119.5 . .
C8 N1 C7 108.09(13) . .
C8 N1 C9 110.75(13) . .
C7 N1 C9 110.21(13) . .
C8 N1 Zn1 116.32(10) . .
C7 N1 Zn1 108.02(10) . .
C9 N1 Zn1 103.33(9) . .
C1 Zn1 C1 117.93(9) . 2_656
C1 Zn1 N1 112.16(6) . .
C1 Zn1 N1 102.31(6) 2_656 .
C1 Zn1 N1 102.31(6) . 2_656
C1 Zn1 N1 112.16(6) 2_656 2_656
N1 Zn1 N1 110.14(7) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.380(2) .
C1 C2 1.386(2) .
C1 Zn1 2.0443(16) .
C2 F1 1.3547(18) .
C2 C3 1.377(2) .
C3 F2 1.3466(18) .
C3 C4 1.379(2) .
C4 F3 1.3400(19) .
C4 C5 1.376(2) .
C5 F4 1.3427(19) .
C5 C6 1.376(2) .
C6 F5 1.3632(18) .
C7 N1 1.483(2) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 N1 1.480(2) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 N1 1.500(2) .
C9 C10 1.512(2) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C15 1.387(2) .
C10 C11 1.393(2) .
C11 C12 1.384(2) .
C11 H11 0.9500 .
C12 C13 1.383(3) .
C12 H12 0.9500 .
C13 C14 1.383(3) .
C13 H13 0.9500 .
C14 C15 1.387(2) .
C14 H14 0.9500 .
C15 H15 0.9500 .
N1 Zn1 2.1626(13) .
Zn1 C1 2.0443(16) 2_656
Zn1 N1 2.1626(13) 2_656
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C8 H8B F5 0.98 2.31 3.164(2) 145.0 .
C7 H7A F2 0.98 2.46 3.174(2) 129.3 2_646
