#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:47:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179306 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/03/4320337.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_4320337
loop_
_publ_author_name
'Jeremy C. Stephens'
'Masood A. Khan'
'Robert P. Houser'
_publ_section_title
;
 Copper(II) Acetate Complexes, [CuLm(OAc)2]n (L = HNPPh3), Stable in the
 Solid State Either as a Dimer (m = 1, n = 2) or a Monomer (m = 2, n = 1)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5064
_journal_page_last               5065
_journal_paper_doi               10.1021/ic0155636
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C40 H38 Cu N2 O4 P2'
_chemical_formula_weight         736.20
_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                109.609(7)
_cell_angle_beta                 103.008(8)
_cell_angle_gamma                99.475(8)
_cell_formula_units_Z            1
_cell_length_a                   8.7983(10)
_cell_length_b                   9.4952(10)
_cell_length_c                   12.5588(13)
_cell_measurement_reflns_used    67
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      20.50
_cell_measurement_theta_min      4.96
_cell_volume                     929.42(19)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4309
_diffrn_reflns_theta_full        26.52
_diffrn_reflns_theta_max         26.52
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.7972
_exptl_absorpt_correction_T_min  0.7053
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             383
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.047(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0415P)²+0.7394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                3273
_reflns_number_total             3562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0155636_s2_1.cif
_cod_data_source_block           bh028b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        929.42(17)
_cod_database_code               4320337
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.0000 0.0000 0.02091(8) Uani 1 2 d S . .
P1 P 0.23870(5) 0.22057(5) 0.26805(3) 0.02110(11) Uani 1 1 d . . .
O1 O 0.18332(16) 0.13937(16) -0.00920(11) 0.0317(3) Uani 1 1 d . . .
O2 O 0.0907(2) 0.17879(19) -0.17483(14) 0.0467(4) Uani 1 1 d . . .
N1 N 0.0954(2) 0.0824(2) 0.16995(13) 0.0299(4) Uani 1 1 d . . .
C1 C 0.4380(2) 0.1887(2) 0.28555(16) 0.0258(4) Uani 1 1 d . . .
C2 C 0.4892(3) 0.1370(3) 0.18533(19) 0.0418(5) Uani 1 1 d . . .
H2A H 0.4214 0.1209 0.1115 0.050 Uiso 1 1 calc R . .
C3 C 0.6400(3) 0.1096(3) 0.1950(2) 0.0511(6) Uani 1 1 d . . .
H3A H 0.6740 0.0773 0.1279 0.061 Uiso 1 1 calc R . .
C4 C 0.7400(3) 0.1299(3) 0.3031(2) 0.0468(6) Uani 1 1 d . . .
H4A H 0.8405 0.1090 0.3088 0.056 Uiso 1 1 calc R . .
C5 C 0.6915(3) 0.1810(3) 0.4026(2) 0.0450(6) Uani 1 1 d . . .
H5A H 0.7601 0.1958 0.4758 0.054 Uiso 1 1 calc R . .
C6 C 0.5415(2) 0.2109(2) 0.39495(18) 0.0342(5) Uani 1 1 d . . .
H6A H 0.5098 0.2457 0.4630 0.041 Uiso 1 1 calc R . .
C7 C 0.2468(2) 0.3955(2) 0.24090(15) 0.0247(4) Uani 1 1 d . . .
C8 C 0.3894(2) 0.5109(2) 0.28184(17) 0.0316(4) Uani 1 1 d . . .
H8A H 0.4854 0.4958 0.3197 0.038 Uiso 1 1 calc R . .
C9 C 0.3891(3) 0.6490(3) 0.2664(2) 0.0449(6) Uani 1 1 d . . .
H9A H 0.4846 0.7268 0.2944 0.054 Uiso 1 1 calc R . .
C10 C 0.2465(4) 0.6704(3) 0.2094(2) 0.0501(6) Uani 1 1 d . . .
H10A H 0.2464 0.7628 0.1989 0.060 Uiso 1 1 calc R . .
C11 C 0.1044(3) 0.5560(3) 0.1680(2) 0.0459(6) Uani 1 1 d . . .
H11A H 0.0089 0.5712 0.1294 0.055 Uiso 1 1 calc R . .
C12 C 0.1035(3) 0.4186(3) 0.18373(18) 0.0352(5) Uani 1 1 d . . .
H12A H 0.0073 0.3416 0.1562 0.042 Uiso 1 1 calc R . .
C13 C 0.2064(2) 0.2607(2) 0.41118(14) 0.0229(4) Uani 1 1 d . . .
C14 C 0.1893(3) 0.1424(2) 0.45349(17) 0.0349(5) Uani 1 1 d . . .
H14A H 0.1990 0.0455 0.4096 0.042 Uiso 1 1 calc R . .
C15 C 0.1580(3) 0.1691(3) 0.56053(18) 0.0394(5) Uani 1 1 d . . .
H15A H 0.1477 0.0901 0.5887 0.047 Uiso 1 1 calc R . .
C16 C 0.1419(3) 0.3121(3) 0.62608(17) 0.0376(5) Uani 1 1 d . . .
H16A H 0.1211 0.3293 0.6982 0.045 Uiso 1 1 calc R . .
C17 C 0.1564(3) 0.4287(3) 0.58484(17) 0.0369(5) Uani 1 1 d . . .
H17A H 0.1439 0.5245 0.6284 0.044 Uiso 1 1 calc R . .
C18 C 0.1899(2) 0.4038(2) 0.47749(16) 0.0291(4) Uani 1 1 d . . .
H18A H 0.2012 0.4836 0.4503 0.035 Uiso 1 1 calc R . .
C19 C 0.3528(3) 0.3205(3) -0.0496(2) 0.0579(8) Uani 1 1 d . . .
H19A H 0.3481 0.3687 -0.1059 0.087 Uiso 1 1 calc R . .
H19B H 0.4381 0.2691 -0.0500 0.087 Uiso 1 1 calc R . .
H19C H 0.3734 0.3980 0.0281 0.087 Uiso 1 1 calc R . .
C20 C 0.1948(2) 0.2044(2) -0.08257(16) 0.0290(4) Uani 1 1 d . . .
H1 H 0.058(3) 0.018(3) 0.194(2) 0.030(6) Uiso 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 0.0033 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
_geom_angle_publ_flag
N1 Cu1 N1 180.00(11) . 2 ?
N1 Cu1 O1 91.23(6) . 2 ?
N1 Cu1 O1 88.77(6) 2 2 ?
N1 Cu1 O1 88.77(6) . . ?
N1 Cu1 O1 91.23(6) 2 . ?
O1 Cu1 O1 180.00(9) 2 . ?
N1 P1 C7 111.21(9) . . ?
N1 P1 C1 115.94(9) . . ?
C7 P1 C1 107.11(9) . . ?
N1 P1 C13 109.60(9) . . ?
C7 P1 C13 106.75(8) . . ?
C1 P1 C13 105.71(8) . . ?
C20 O1 Cu1 131.62(12) . . ?
P1 N1 Cu1 138.01(11) . . ?
C6 C1 C2 118.64(19) . . ?
C6 C1 P1 122.64(15) . . ?
C2 C1 P1 118.70(15) . . ?
C3 C2 C1 120.4(2) . . ?
C4 C3 C2 120.4(2) . . ?
C5 C4 C3 119.9(2) . . ?
C4 C5 C6 120.6(2) . . ?
C5 C6 C1 120.1(2) . . ?
C8 C7 C12 119.64(19) . . ?
C8 C7 P1 121.59(15) . . ?
C12 C7 P1 118.64(15) . . ?
C7 C8 C9 120.0(2) . . ?
C10 C9 C8 119.8(2) . . ?
C11 C10 C9 120.4(2) . . ?
C10 C11 C12 120.1(2) . . ?
C11 C12 C7 119.9(2) . . ?
C18 C13 C14 119.01(17) . . ?
C18 C13 P1 121.67(15) . . ?
C14 C13 P1 119.24(14) . . ?
C15 C14 C13 120.1(2) . . ?
C16 C15 C14 120.5(2) . . ?
C17 C16 C15 120.00(19) . . ?
C16 C17 C18 120.0(2) . . ?
C13 C18 C17 120.35(19) . . ?
O2 C20 O1 126.01(18) . . ?
O2 C20 C19 118.94(19) . . ?
O1 C20 C19 115.05(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.9309(15) . ?
Cu1 N1 1.9309(15) 2 ?
Cu1 O1 1.9621(13) 2 ?
Cu1 O1 1.9621(13) . ?
P1 N1 1.5811(15) . ?
P1 C7 1.798(2) . ?
P1 C1 1.8056(19) . ?
P1 C13 1.8065(17) . ?
O1 C20 1.282(2) . ?
O2 C20 1.225(2) . ?
C1 C6 1.393(3) . ?
C1 C2 1.393(3) . ?
C2 C3 1.380(3) . ?
C3 C4 1.373(4) . ?
C4 C5 1.371(4) . ?
C5 C6 1.384(3) . ?
C7 C8 1.385(3) . ?
C7 C12 1.394(3) . ?
C8 C9 1.389(3) . ?
C9 C10 1.380(4) . ?
C10 C11 1.376(4) . ?
C11 C12 1.383(3) . ?
C13 C18 1.386(3) . ?
C13 C14 1.395(3) . ?
C14 C15 1.382(3) . ?
C15 C16 1.381(3) . ?
C16 C17 1.371(3) . ?
C17 C18 1.396(3) . ?
C19 C20 1.500(3) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Cu1 O1 C20 -150.27(18) . . . . ?
N1 Cu1 O1 C20 29.73(18) 2 . . . ?
O1 Cu1 O1 C20 -29(100) 2 . . . ?
C7 P1 N1 Cu1 41.97(19) . . . . ?
C1 P1 N1 Cu1 -80.70(19) . . . . ?
C13 P1 N1 Cu1 159.77(15) . . . . ?
N1 Cu1 N1 P1 -62(40) 2 . . . ?
O1 Cu1 N1 P1 -170.08(17) 2 . . . ?
O1 Cu1 N1 P1 9.92(17) . . . . ?
N1 P1 C1 C6 -127.83(17) . . . . ?
C7 P1 C1 C6 107.37(18) . . . . ?
C13 P1 C1 C6 -6.2(2) . . . . ?
N1 P1 C1 C2 50.9(2) . . . . ?
C7 P1 C1 C2 -73.88(19) . . . . ?
C13 P1 C1 C2 172.56(18) . . . . ?
C6 C1 C2 C3 -0.4(4) . . . . ?
P1 C1 C2 C3 -179.2(2) . . . . ?
C1 C2 C3 C4 1.3(4) . . . . ?
C2 C3 C4 C5 -1.5(4) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C4 C5 C6 C1 0.1(4) . . . . ?
C2 C1 C6 C5 -0.3(3) . . . . ?
P1 C1 C6 C5 178.46(18) . . . . ?
N1 P1 C7 C8 -154.26(16) . . . . ?
C1 P1 C7 C8 -26.63(18) . . . . ?
C13 P1 C7 C8 86.23(17) . . . . ?
N1 P1 C7 C12 29.84(18) . . . . ?
C1 P1 C7 C12 157.46(15) . . . . ?
C13 P1 C7 C12 -89.67(16) . . . . ?
C12 C7 C8 C9 0.3(3) . . . . ?
P1 C7 C8 C9 -175.55(16) . . . . ?
C7 C8 C9 C10 -0.5(3) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C10 C11 C12 C7 -0.4(3) . . . . ?
C8 C7 C12 C11 0.1(3) . . . . ?
P1 C7 C12 C11 176.13(16) . . . . ?
N1 P1 C13 C18 -119.45(16) . . . . ?
C7 P1 C13 C18 1.10(17) . . . . ?
C1 P1 C13 C18 114.91(16) . . . . ?
N1 P1 C13 C14 57.20(18) . . . . ?
C7 P1 C13 C14 177.74(15) . . . . ?
C1 P1 C13 C14 -68.44(17) . . . . ?
C18 C13 C14 C15 -0.6(3) . . . . ?
P1 C13 C14 C15 -177.36(17) . . . . ?
C13 C14 C15 C16 0.6(3) . . . . ?
C14 C15 C16 C17 0.2(3) . . . . ?
C15 C16 C17 C18 -1.0(3) . . . . ?
C14 C13 C18 C17 -0.1(3) . . . . ?
P1 C13 C18 C17 176.54(15) . . . . ?
C16 C17 C18 C13 0.9(3) . . . . ?
Cu1 O1 C20 O2 -8.4(3) . . . . ?
Cu1 O1 C20 C19 172.30(17) . . . . ?
