#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:03:17 +0100 (vie 25 de mar de 2016) $
#$Revision: 179823 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/19/7011968.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_7011968
loop_
_publ_author_name
'Vetrichelvan, Muthalagu'
'Lai, Yee-Hing'
'Fun Mok, Kum'
_publ_section_title
;
 A new NS4 quinquedentate macrocyclic ligand: synthesis, structure and
 properties of its Ni(ii), Pd(ii), Pt(ii), Cu(ii), Cu(i) and Ag(i)
 complexesPresented at ISMC-2001 held in Fukuoka, Japan from July
 15--20, 2001.Electronic supplementary information (ESI) available:
 synthetic scheme for macrocyclic complexes 12--17; views of 12, 15 and
 16; cyclic voltammograms of 13 and 14. See
 http://www.rsc.org/suppdata/dt/b2/b206182a/
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              295
_journal_paper_doi               10.1039/b206182a
_journal_year                    2003
_chemical_formula_sum            'C19 H23 Cu F6 N P S4'
_chemical_formula_weight         602.13
_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                105.621(1)
_cell_angle_beta                 101.527(1)
_cell_angle_gamma                113.172(1)
_cell_formula_units_Z            2
_cell_length_a                   9.2285(2)
_cell_length_b                   11.6204(2)
_cell_length_c                   13.0124(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1159.45(5)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9662
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.428
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            'Very pale yellow'
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Prismatic fragment'
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0536
_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)+(0.0740P)²+0.9661P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                3294
_reflns_number_total             4705
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206182a.txt
_cod_data_source_block           kf22
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1159.45(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011968
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
Cu Cu 0.55523(8) 0.74359(6) 0.43344(5) 0.0530(2) Uani 1 1 d . . .
C1 C 0.9141(6) 0.9169(5) 0.6430(4) 0.0539(12) Uani 1 1 d . . .
H1A H 0.9974 0.9053 0.6914 0.065 Uiso 1 1 calc R . .
H1B H 0.9639 1.0116 0.6530 0.065 Uiso 1 1 calc R . .
S2 S 0.86887(15) 0.81580(12) 0.49723(10) 0.0492(3) Uani 1 1 d . . .
C3 C 0.8338(6) 0.6542(5) 0.5086(4) 0.0493(11) Uani 1 1 d . . .
H3A H 0.9404 0.6550 0.5350 0.059 Uiso 1 1 calc R . .
H3B H 0.7770 0.6395 0.5626 0.059 Uiso 1 1 calc R . .
C4 C 0.7281(6) 0.5430(5) 0.3934(4) 0.0506(11) Uani 1 1 d . . .
H4A H 0.7251 0.4590 0.3947 0.061 Uiso 1 1 calc R . .
H4B H 0.7785 0.5651 0.3380 0.061 Uiso 1 1 calc R . .
S5 S 0.51513(14) 0.51931(11) 0.35086(9) 0.0429(3) Uani 1 1 d . . .
C6 C 0.4647(6) 0.4651(5) 0.1969(4) 0.0492(11) Uani 1 1 d . . .
H6A H 0.4774 0.3846 0.1694 0.059 Uiso 1 1 calc R . .
H6B H 0.3476 0.4396 0.1623 0.059 Uiso 1 1 calc R . .
C7 C 0.5688(5) 0.5683(4) 0.1573(3) 0.0431(10) Uani 1 1 d . . .
C8 C 0.7027(6) 0.5585(5) 0.1304(4) 0.0532(12) Uani 1 1 d . . .
H8A H 0.7243 0.4885 0.1368 0.064 Uiso 1 1 calc R . .
C9 C 0.8047(6) 0.6512(6) 0.0943(4) 0.0636(14) Uani 1 1 d . . .
H9A H 0.8939 0.6432 0.0766 0.076 Uiso 1 1 calc R . .
C10 C 0.7739(7) 0.7542(6) 0.0848(4) 0.0660(15) Uani 1 1 d . . .
H10A H 0.8435 0.8177 0.0621 0.079 Uiso 1 1 calc R . .
C11 C 0.6399(7) 0.7637(5) 0.1090(4) 0.0570(13) Uani 1 1 d . . .
H11A H 0.6187 0.8334 0.1013 0.068 Uiso 1 1 calc R . .
C12 C 0.5356(5) 0.6719(4) 0.1446(3) 0.0440(10) Uani 1 1 d . . .
C13 C 0.3915(6) 0.6883(5) 0.1686(4) 0.0523(11) Uani 1 1 d . . .
H13A H 0.3096 0.6047 0.1688 0.063 Uiso 1 1 calc R . .
H13B H 0.3369 0.7098 0.1102 0.063 Uiso 1 1 calc R . .
S14 S 0.47235(15) 0.82549(11) 0.30718(10) 0.0466(3) Uani 1 1 d . . .
C15 C 0.2816(6) 0.8264(5) 0.3215(5) 0.0583(13) Uani 1 1 d . . .
H15A H 0.3127 0.9064 0.3872 0.070 Uiso 1 1 calc R . .
H15B H 0.2251 0.8355 0.2552 0.070 Uiso 1 1 calc R . .
C16 C 0.1573(6) 0.7039(5) 0.3344(4) 0.0543(12) Uani 1 1 d . . .
H16A H 0.1055 0.6277 0.2617 0.065 Uiso 1 1 calc R . .
H16B H 0.0693 0.7224 0.3516 0.065 Uiso 1 1 calc R . .
S17 S 0.24083(15) 0.65305(12) 0.44178(10) 0.0499(3) Uani 1 1 d . . .
C18 C 0.3224(6) 0.8025(5) 0.5710(4) 0.0583(13) Uani 1 1 d . . .
H18A H 0.3365 0.8798 0.5509 0.070 Uiso 1 1 calc R . .
H18B H 0.2411 0.7885 0.6097 0.070 Uiso 1 1 calc R . .
C19 C 0.4881(5) 0.8342(4) 0.6512(4) 0.0437(10) Uani 1 1 d . . .
C20 C 0.5131(7) 0.8657(5) 0.7658(4) 0.0562(12) Uani 1 1 d . . .
H20A H 0.4257 0.8612 0.7928 0.067 Uiso 1 1 calc R . .
C21 C 0.6670(7) 0.9036(5) 0.8387(4) 0.0608(13) Uani 1 1 d . . .
H21A H 0.6849 0.9223 0.9157 0.073 Uiso 1 1 calc R . .
C22 C 0.7952(6) 0.9140(5) 0.7974(4) 0.0530(12) Uani 1 1 d . . .
H22A H 0.9011 0.9401 0.8462 0.064 Uiso 1 1 calc R . .
C23 C 0.7660(6) 0.8854(4) 0.6835(4) 0.0444(10) Uani 1 1 d . . .
N24 N 0.6124(4) 0.8398(3) 0.6089(3) 0.0408(8) Uani 1 1 d . . .
P P -0.10106(16) 0.26983(13) 0.13104(11) 0.0501(3) Uani 1 1 d . . .
F1 F 0.0855(5) 0.3348(5) 0.2133(4) 0.1247(16) Uani 1 1 d . . .
F2 F -0.0575(6) 0.1913(4) 0.0371(4) 0.142(2) Uani 1 1 d . . .
F3 F -0.2863(5) 0.2099(5) 0.0546(4) 0.1149(15) Uani 1 1 d . . .
F4 F -0.1395(5) 0.3529(4) 0.2295(4) 0.1076(13) Uani 1 1 d . . .
F5 F -0.1587(5) 0.1478(4) 0.1707(4) 0.1118(15) Uani 1 1 d . . .
F6 F -0.0434(5) 0.3948(4) 0.0935(4) 0.1051(13) 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 0.0033 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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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'
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
N24 Cu S14 122.05(10) . . ?
N24 Cu S5 122.00(10) . . ?
S14 Cu S5 114.65(4) . . ?
N24 Cu S2 82.09(10) . . ?
S14 Cu S2 114.31(5) . . ?
S5 Cu S2 85.77(4) . . ?
N24 Cu S17 80.27(10) . . ?
S14 Cu S17 86.43(4) . . ?
S5 Cu S17 92.43(4) . . ?
S2 Cu S17 157.94(4) . . ?
C23 C1 S2 115.8(3) . . ?
C1 S2 C3 100.1(2) . . ?
C1 S2 Cu 95.41(16) . . ?
C3 S2 Cu 92.59(15) . . ?
C4 C3 S2 108.3(3) . . ?
C3 C4 S5 111.5(3) . . ?
C4 S5 C6 100.0(2) . . ?
C4 S5 Cu 102.66(15) . . ?
C6 S5 Cu 111.05(15) . . ?
C7 C6 S5 115.6(3) . . ?
C8 C7 C12 118.7(4) . . ?
C8 C7 C6 118.1(4) . . ?
C12 C7 C6 123.1(4) . . ?
C9 C8 C7 121.1(5) . . ?
C10 C9 C8 119.9(5) . . ?
C9 C10 C11 119.7(5) . . ?
C10 C11 C12 121.5(5) . . ?
C11 C12 C7 119.1(4) . . ?
C11 C12 C13 118.3(4) . . ?
C7 C12 C13 122.6(4) . . ?
C12 C13 S14 108.3(3) . . ?
C15 S14 C13 101.6(2) . . ?
C15 S14 Cu 105.90(16) . . ?
C13 S14 Cu 104.82(15) . . ?
C16 C15 S14 116.6(3) . . ?
C15 C16 S17 116.3(3) . . ?
C16 S17 C18 102.2(2) . . ?
C16 S17 Cu 97.20(16) . . ?
C18 S17 Cu 88.26(16) . . ?
C19 C18 S17 112.8(3) . . ?
N24 C19 C20 122.0(4) . . ?
N24 C19 C18 118.2(4) . . ?
C20 C19 C18 119.7(4) . . ?
C21 C20 C19 119.3(5) . . ?
C20 C21 C22 119.3(4) . . ?
C21 C22 C23 119.5(5) . . ?
N24 C23 C22 122.2(4) . . ?
N24 C23 C1 119.3(4) . . ?
C22 C23 C1 118.3(4) . . ?
C23 N24 C19 117.6(4) . . ?
C23 N24 Cu 120.9(3) . . ?
C19 N24 Cu 120.3(3) . . ?
F2 P F3 93.6(3) . . ?
F2 P F5 90.7(3) . . ?
F3 P F5 88.3(2) . . ?
F2 P F4 178.2(3) . . ?
F3 P F4 88.2(3) . . ?
F5 P F4 89.7(2) . . ?
F2 P F1 89.1(3) . . ?
F3 P F1 177.3(3) . . ?
F5 P F1 91.7(2) . . ?
F4 P F1 89.2(3) . . ?
F2 P F6 90.6(2) . . ?
F3 P F6 91.7(2) . . ?
F5 P F6 178.7(2) . . ?
F4 P F6 89.0(2) . . ?
F1 P F6 88.1(2) . . ?
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
Cu N24 2.103(3) . ?
Cu S14 2.2590(12) . ?
Cu S5 2.3786(12) . ?
Cu S2 2.5542(13) . ?
Cu S17 2.7059(14) . ?
C1 C23 1.509(6) . ?
C1 S2 1.803(5) . ?
S2 C3 1.829(5) . ?
C3 C4 1.499(6) . ?
C4 S5 1.818(5) . ?
S5 C6 1.828(4) . ?
C6 C7 1.501(6) . ?
C7 C8 1.387(6) . ?
C7 C12 1.395(6) . ?
C8 C9 1.385(7) . ?
C9 C10 1.364(8) . ?
C10 C11 1.373(7) . ?
C11 C12 1.385(6) . ?
C12 C13 1.495(6) . ?
C13 S14 1.824(5) . ?
S14 C15 1.811(5) . ?
C15 C16 1.514(7) . ?
C16 S17 1.808(5) . ?
S17 C18 1.818(5) . ?
C18 C19 1.509(6) . ?
C19 N24 1.355(5) . ?
C19 C20 1.384(6) . ?
C20 C21 1.363(7) . ?
C21 C22 1.371(7) . ?
C22 C23 1.373(6) . ?
C23 N24 1.347(5) . ?
P F2 1.540(4) . ?
P F3 1.552(4) . ?
P F5 1.572(4) . ?
P F4 1.576(4) . ?
P F1 1.576(4) . ?
P F6 1.584(4) . ?
