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#$Date: 2016-03-21 10:20:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178646 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/57/4075757.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_4075757
loop_
_publ_author_name
'Pampaloni, Guido'
'Peloso, Riccardo'
'Graiff, Claudia'
'Tiripicchio, Antonio'
_publ_section_title
;
 Olefin Trifluoroacetato Derivatives of Copper(I) and Their Olefin/CO
 Exchange Reactions
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              819
_journal_paper_doi               10.1021/om049314b
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C12 H12 Cu2 F6 O4'
_chemical_formula_weight         461.30
_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                 94.89(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.606(5)
_cell_length_b                   11.067(5)
_cell_length_c                   11.864(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      40
_cell_measurement_theta_min      20
_cell_volume                     1518.3(11)
_computing_molecular_graphics    'ORTEP 3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ENRAF NONIUS CAD 4'
_diffrn_measurement_method       'θ/2θ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3014
_diffrn_reflns_theta_full        70.01
_diffrn_reflns_theta_max         70.01
_diffrn_reflns_theta_min         5.12
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    4.276
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.432
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Parkin & al (1995)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.813
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0704P)²+4.2316P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                2537
_reflns_number_total             2872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049314bsi20041230_114344.cif
_cod_data_source_block           ricban
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4075757
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
C1 C 0.1982(3) 0.3289(3) -0.0026(3) 0.0240(6) Uani 1 1 d .
C2 C 0.1276(3) 0.3919(3) -0.1010(3) 0.0284(7) Uani 1 1 d .
C3 C 0.4866(3) 0.3464(3) 0.1732(2) 0.0227(6) Uani 1 1 d .
C4 C 0.5947(3) 0.4287(3) 0.1794(3) 0.0254(6) Uani 1 1 d .
C5 C 0.1330(3) 0.2148(3) 0.3238(3) 0.0286(7) Uani 1 1 d .
H5 H 0.1315 0.1542 0.2694 0.034 Uiso 1 1 calc R
C6 C 0.2365(3) 0.2185(3) 0.3903(3) 0.0292(7) Uani 1 1 d .
H6 H 0.2881 0.1597 0.3701 0.035 Uiso 1 1 calc R
C7 C 0.2856(4) 0.2946(3) 0.4874(3) 0.0432(9) Uani 1 1 d .
H7A H 0.2727 0.2507 0.5560 0.052 Uiso 1 1 calc R
H7B H 0.3686 0.2970 0.4829 0.052 Uiso 1 1 calc R
C8 C 0.2522(4) -0.0786(3) -0.0047(3) 0.0472(10) Uani 1 1 d .
H8A H 0.1932 -0.0375 -0.0533 0.057 Uiso 1 1 calc R
H8B H 0.3225 -0.0797 -0.0434 0.057 Uiso 1 1 calc R
C9 C 0.2742(3) -0.0076(3) 0.1050(3) 0.0281(6) Uani 1 1 d .
H9 H 0.2149 0.0389 0.1304 0.034 Uiso 1 1 calc R
C10 C 0.3798(2) -0.0107(3) 0.1674(2) 0.0218(6) Uani 1 1 d .
H10 H 0.3902 0.0352 0.2331 0.026 Uiso 1 1 calc R
C11 C 0.4790(3) -0.0861(3) 0.1327(3) 0.0275(6) Uani 1 1 d .
H11A H 0.5513 -0.0469 0.1582 0.033 Uiso 1 1 calc R
H11B H 0.4747 -0.0908 0.0508 0.033 Uiso 1 1 calc R
C12 C 0.0216(3) 0.2860(3) 0.3186(3) 0.0299(7) Uani 1 1 d .
H12A H -0.0338 0.2388 0.3567 0.036 Uiso 1 1 calc R
H12B H -0.0077 0.2912 0.2397 0.036 Uiso 1 1 calc R
Cu1 Cu 0.35781(4) 0.14853(4) 0.08258(4) 0.02350(14) Uani 1 1 d .
Cu2 Cu 0.25400(4) 0.30294(4) 0.23853(4) 0.02438(14) Uani 1 1 d .
F1 F 0.02473(19) 0.3370(2) -0.1204(2) 0.0507(6) Uani 1 1 d .
F2 F 0.17852(18) 0.3873(2) -0.19759(15) 0.0388(5) Uani 1 1 d .
F3 F 0.1071(2) 0.50736(19) -0.08048(18) 0.0443(5) Uani 1 1 d .
F4 F 0.6137(2) 0.4702(2) 0.07752(19) 0.0521(6) Uani 1 1 d .
F5 F 0.58545(18) 0.52273(19) 0.2462(2) 0.0447(5) Uani 1 1 d .
F6 F 0.68843(17) 0.36853(19) 0.2180(2) 0.0457(6) Uani 1 1 d .
O1 O 0.2629(2) 0.2464(2) -0.02989(19) 0.0316(5) Uani 1 1 d .
O2 O 0.1792(2) 0.3657(2) 0.09273(19) 0.0367(6) Uani 1 1 d .
O3 O 0.49150(19) 0.25744(19) 0.10937(19) 0.0276(5) Uani 1 1 d .
O4 O 0.40832(19) 0.3786(2) 0.23150(19) 0.0294(5) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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 C1 O2 129.6(3) . .
O1 C1 C2 115.5(3) . .
O2 C1 C2 114.8(3) . .
F3 C2 F2 107.1(3) . .
F3 C2 F1 107.3(3) . .
F2 C2 F1 106.7(3) . .
F3 C2 C1 113.0(3) . .
F2 C2 C1 112.9(3) . .
F1 C2 C1 109.5(3) . .
O3 C3 O4 129.7(3) . .
O3 C3 C4 114.5(3) . .
O4 C3 C4 115.8(3) . .
F5 C4 F6 107.2(3) . .
F5 C4 F4 107.6(3) . .
F6 C4 F4 107.1(3) . .
F5 C4 C3 112.7(3) . .
F6 C4 C3 111.1(2) . .
F4 C4 C3 111.0(2) . .
C6 C5 C12 135.0(3) . .
C6 C5 Cu2 70.64(18) . .
C12 C5 Cu2 110.6(2) . .
C5 C6 C7 135.3(3) . .
C5 C6 Cu2 70.03(19) . .
C7 C6 Cu2 111.0(2) . .
C8 C7 C6 122.5(3) 2 .
C7 C8 C9 113.5(3) 2_545 .
C10 C9 C8 121.5(3) . .
C10 C9 Cu1 71.02(18) . .
C8 C9 Cu1 112.2(2) . .
C9 C10 C11 122.2(3) . .
C9 C10 Cu1 69.17(17) . .
C11 C10 Cu1 114.3(2) . .
C10 C11 C12 112.4(2) . 2_545
C5 C12 C11 119.9(3) . 2
O3 Cu1 O1 99.16(10) . .
O3 Cu1 C9 152.55(11) . .
O1 Cu1 C9 108.20(12) . .
O3 Cu1 C10 112.74(11) . .
O1 Cu1 C10 147.86(11) . .
C9 Cu1 C10 39.81(12) . .
O3 Cu1 Cu2 84.22(7) . .
O1 Cu1 Cu2 82.43(7) . .
C9 Cu1 Cu2 101.15(10) . .
C10 Cu1 Cu2 103.87(9) . .
O4 Cu2 O2 98.29(11) . .
O4 Cu2 C5 151.79(12) . .
O2 Cu2 C5 109.19(13) . .
O4 Cu2 C6 112.70(13) . .
O2 Cu2 C6 148.32(12) . .
C5 Cu2 C6 39.33(14) . .
O4 Cu2 Cu1 78.09(7) . .
O2 Cu2 Cu1 79.82(8) . .
C5 Cu2 Cu1 112.30(9) . .
C6 Cu2 Cu1 111.96(9) . .
C1 O1 Cu1 122.7(2) . .
C1 O2 Cu2 125.4(2) . .
C3 O3 Cu1 120.4(2) . .
C3 O4 Cu2 127.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.243(4) .
C1 O2 1.240(4) .
C1 C2 1.535(4) .
C2 F3 1.325(4) .
C2 F2 1.335(4) .
C2 F1 1.342(4) .
C3 O3 1.246(4) .
C3 O4 1.240(4) .
C3 C4 1.547(4) .
C4 F5 1.319(4) .
C4 F6 1.323(4) .
C4 F4 1.329(4) .
C5 C6 1.380(5) .
C5 C12 1.512(4) .
C5 Cu2 2.047(3) .
C6 C7 1.500(5) .
C6 Cu2 2.054(3) .
C7 C8 1.490(5) 2
C8 C7 1.490(5) 2_545
C8 C9 1.523(5) .
C9 C10 1.377(4) .
C9 Cu1 2.011(3) .
C10 C11 1.508(4) .
C10 Cu1 2.034(3) .
C11 C12 1.529(4) 2_545
C12 C11 1.529(4) 2
Cu1 O3 1.969(2) .
Cu1 O1 1.979(2) .
Cu1 Cu2 2.8592(12) .
Cu2 O4 1.985(2) .
Cu2 O2 1.993(2) .
