#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:44:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179202 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/37/4313786.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_4313786
loop_
_publ_author_name
'Subrata Kumar Dey'
'Bappaditya Bag'
'K. M. Abdul Malik'
'M. Salah El Fallah'
'Joan Ribas'
'Samiran Mitra'
_publ_section_title
;
 A Quasi-Tetrahedral Cu4 Cluster and a Helical-Chain Copper(II) Complex
 with Single Syn-Anti Carboxylate Bridges: Crystal Structure and Magnetic
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4029
_journal_page_last               4035
_journal_paper_doi               10.1021/ic0206488
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C15 H9 Cu F3 N2 O4'
_chemical_formula_weight         401.78
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.419(2)
_cell_length_b                   16.289(5)
_cell_length_c                   8.937(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      16
_cell_volume                     1443.9(9)
_computing_cell_refinement       'CAD4 Express software (Nonius, 1994)'
_computing_data_collection       'CAD4 Express software (Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Wocadlo & Harms, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius CAD4 diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2839
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.574
_exptl_absorpt_correction_T_max  0.6496
_exptl_absorpt_correction_T_min  0.6088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    'calculated positions, riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0431
_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)+(0.0731P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                2035
_reflns_number_total             2628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0206488.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4313786
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.10056(4) 0.16351(3) 0.33355(5) 0.01552(16) Uani 1 1 d . . .
O1 O 0.0638(3) 0.22759(16) 0.4949(3) 0.0231(6) Uani 1 1 d . . .
O2 O -0.0505(3) 0.27888(16) 0.6438(3) 0.0233(6) Uani 1 1 d . . .
O3 O 0.2670(3) 0.22154(16) 0.3503(3) 0.0221(6) Uani 1 1 d . . .
O4 O 0.1984(3) 0.35366(16) 0.3156(3) 0.0267(7) Uani 1 1 d . . .
N1 N 0.1645(3) 0.07033(19) 0.2272(3) 0.0176(7) Uani 1 1 d . . .
N2 N -0.0363(3) 0.07939(18) 0.3448(3) 0.0150(6) Uani 1 1 d . . .
C1 C 0.2629(4) 0.0703(2) 0.1613(4) 0.0230(9) Uani 1 1 d . . .
H1 H 0.3159 0.1183 0.1670 0.028 Uiso 1 1 calc R . .
C2 C 0.2900(4) 0.0011(2) 0.0836(4) 0.0250(9) Uani 1 1 d . . .
H2 H 0.3612 0.0021 0.0380 0.030 Uiso 1 1 calc R . .
C3 C 0.2131(4) -0.0684(2) 0.0736(4) 0.0231(9) Uani 1 1 d . . .
H3 H 0.2301 -0.1157 0.0204 0.028 Uiso 1 1 calc R . .
C4 C 0.1102(4) -0.0687(2) 0.1421(4) 0.0207(8) Uani 1 1 d . . .
H4 H 0.0557 -0.1159 0.1371 0.025 Uiso 1 1 calc R . .
C5 C 0.0892(4) 0.0019(2) 0.2182(4) 0.0164(7) Uani 1 1 d . . .
C6 C -0.0190(4) 0.0099(2) 0.2884(4) 0.0167(8) Uani 1 1 d . . .
H6 H -0.0753 -0.0355 0.2921 0.020 Uiso 1 1 calc R . .
C7 C -0.1489(3) 0.0949(2) 0.4000(4) 0.0167(8) Uani 1 1 d . . .
C8 C -0.2584(4) 0.0421(2) 0.3614(5) 0.0227(9) Uani 1 1 d . . .
H8 H -0.2572 -0.0052 0.2997 0.027 Uiso 1 1 calc R . .
C9 C -0.3698(4) 0.0571(3) 0.4114(5) 0.0267(9) Uani 1 1 d . . .
H9 H -0.4441 0.0203 0.3838 0.032 Uiso 1 1 calc R . .
C10 C -0.3725(4) 0.1256(2) 0.5012(5) 0.0248(9) Uani 1 1 d . . .
H10 H -0.4486 0.1364 0.5356 0.030 Uiso 1 1 calc R . .
C11 C -0.2629(4) 0.1784(2) 0.5407(4) 0.0227(9) Uani 1 1 d . . .
H11 H -0.2647 0.2250 0.6040 0.027 Uiso 1 1 calc R . .
C12 C -0.1501(4) 0.1655(2) 0.4908(4) 0.0162(7) Uani 1 1 d . . .
C13 C -0.0373(4) 0.2274(2) 0.5462(4) 0.0183(8) Uani 1 1 d . . .
C14 C 0.2789(4) 0.2982(2) 0.3334(4) 0.0189(8) Uani 1 1 d . . .
C15 C 0.4247(4) 0.3221(2) 0.3431(6) 0.0308(10) Uani 1 1 d . . .
F1 F 0.5024(3) 0.3268(2) 0.4933(4) 0.0641(9) Uani 1 1 d . . .
F2 F 0.4851(3) 0.26836(17) 0.2750(4) 0.0463(7) Uani 1 1 d . . .
F3 F 0.4330(3) 0.39331(18) 0.2789(5) 0.0807(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'
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'
Cu Cu 0.3201 1.2651 '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'
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
O1 Cu1 O3 93.25(11) . . ?
O1 Cu1 N2 91.47(11) . . ?
O3 Cu1 N2 164.38(12) . . ?
O1 Cu1 N1 160.26(12) . . ?
O3 Cu1 N1 89.21(12) . . ?
N2 Cu1 N1 81.45(12) . . ?
O1 Cu1 O2 95.14(12) . 4_565 ?
O3 Cu1 O2 105.65(11) . 4_565 ?
N2 Cu1 O2 88.72(11) . 4_565 ?
N1 Cu1 O2 103.05(11) . 4_565 ?
C13 O1 Cu1 130.6(2) . . ?
C13 O2 Cu1 129.5(2) . 4_566 ?
C14 O3 Cu1 126.0(2) . . ?
C1 N1 C5 119.1(3) . . ?
C1 N1 Cu1 128.5(3) . . ?
C5 N1 Cu1 112.3(2) . . ?
C6 N2 C7 121.7(3) . . ?
C6 N2 Cu1 113.5(2) . . ?
C7 N2 Cu1 124.7(2) . . ?
N1 C1 C2 121.4(4) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 119.2(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 118.2(4) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
N1 C5 C4 122.5(3) . . ?
N1 C5 C6 114.4(3) . . ?
C4 C5 C6 123.0(3) . . ?
N2 C6 C5 118.2(3) . . ?
N2 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C8 C7 C12 119.8(3) . . ?
C8 C7 N2 120.4(3) . . ?
C12 C7 N2 119.8(3) . . ?
C7 C8 C9 121.2(4) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C10 C9 C8 119.9(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 119.2(3) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C10 C11 C12 122.3(4) . . ?
C10 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C11 C12 C7 117.7(3) . . ?
C11 C12 C13 116.2(3) . . ?
C7 C12 C13 126.1(3) . . ?
O2 C13 O1 122.1(3) . . ?
O2 C13 C12 115.8(3) . . ?
O1 C13 C12 122.0(3) . . ?
O4 C14 O3 131.5(4) . . ?
O4 C14 C15 116.7(3) . . ?
O3 C14 C15 111.8(3) . . ?
F3 C15 F2 106.2(4) . . ?
F3 C15 F1 106.7(4) . . ?
F2 C15 F1 105.8(4) . . ?
F3 C15 C14 113.2(3) . . ?
F2 C15 C14 113.8(4) . . ?
F1 C15 C14 110.6(4) . . ?
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 O1 1.911(3) . ?
Cu1 O3 1.940(3) . ?
Cu1 N2 2.002(3) . ?
Cu1 N1 2.010(3) . ?
Cu1 O2 2.144(3) 4_565 ?
O1 C13 1.271(4) . ?
O2 C13 1.248(4) . ?
O2 Cu1 2.144(3) 4_566 ?
O3 C14 1.268(5) . ?
O4 C14 1.210(4) . ?
N1 C1 1.329(5) . ?
N1 C5 1.351(5) . ?
N2 C6 1.274(5) . ?
N2 C7 1.427(4) . ?
C1 C2 1.397(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.374(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.454(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(5) . ?
C7 C12 1.409(5) . ?
C8 C9 1.386(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.513(5) . ?
C14 C15 1.545(5) . ?
C15 F3 1.309(5) . ?
C15 F2 1.328(5) . ?
C15 F1 1.341(6) . ?
