#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:34:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180227 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/13/7111359.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111359
loop_
_publ_author_name
'Fielden, John'
'Long, De-Liang'
'Cronin, Leroy'
_publ_section_title
;
 Secondary coordination sphere controlled reversible geometry
 reorganisations in copper(ii) complexes
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              2156
_journal_page_last               2157
_journal_paper_doi               10.1039/b407229d
_journal_year                    2004
_chemical_formula_moiety         'C12 H28 Cu N4 O2 2+), 2(F 1-), 2(H2 O)'
_chemical_formula_sum            'C12 H32 Cu F2 N4 O4'
_chemical_formula_weight         397.96
_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                108.5670(10)
_cell_angle_beta                 92.2330(10)
_cell_angle_gamma                112.9120(10)
_cell_formula_units_Z            1
_cell_length_a                   7.0993(2)
_cell_length_b                   7.1315(2)
_cell_length_c                   10.0059(3)
_cell_measurement_reflns_used    5333
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.5
_cell_volume                     434.56(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       ω
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7086
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  1.045
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             211
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.28
_refine_diff_density_rms         0.05
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1974
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0197
_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)+(0.0208P)²+0.2299P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0524
_reflns_number_gt                1942
_reflns_number_total             1974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b407229dsup1.cif
_cod_data_source_block           JF243RR_anti
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               7111359
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
Cu Cu 0.0000 0.0000 0.0000 0.01128(7) Uani 1 2 d S
N1 N 0.09146(16) -0.10552(17) 0.14456(11) 0.0142(2) Uani 1 1 d .
H1A H -0.0163 -0.2290 0.1401 0.017 Uiso 1 1 calc R
H1B H 0.1942 -0.1428 0.1146 0.017 Uiso 1 1 calc R
N2 N -0.13083(16) 0.15708(17) 0.14370(11) 0.0144(2) Uani 1 1 d .
H2A H -0.1452 0.2575 0.1132 0.017 Uiso 1 1 calc R
H2B H -0.2600 0.0590 0.1392 0.017 Uiso 1 1 calc R
C1 C 0.16590(19) 0.0389(2) 0.29894(13) 0.0156(2) Uani 1 1 d .
H1C H 0.1919 -0.0449 0.3526 0.019 Uiso 1 1 calc R
C2 C 0.0009(2) 0.1114(2) 0.35891(14) 0.0177(3) Uani 1 1 d .
H2C H -0.1303 -0.0162 0.3371 0.021 Uiso 1 1 calc R
H2D H 0.0414 0.1808 0.4625 0.021 Uiso 1 1 calc R
C3 C -0.02962(19) 0.2697(2) 0.29779(13) 0.0152(2) Uani 1 1 d .
H3 H -0.1215 0.3257 0.3507 0.018 Uiso 1 1 calc R
C4 C 0.1768(2) 0.4640(2) 0.31543(14) 0.0171(3) Uani 1 1 d .
H4A H 0.1531 0.5528 0.2667 0.020 Uiso 1 1 calc R
H4B H 0.2267 0.5533 0.4166 0.020 Uiso 1 1 calc R
C5 C 0.34390(19) 0.3954(2) 0.25593(13) 0.0155(2) Uani 1 1 d .
H5 H 0.3032 0.3248 0.1513 0.019 Uiso 1 1 calc R
C6 C 0.37018(19) 0.2358(2) 0.31807(14) 0.0173(3) Uani 1 1 d .
H6A H 0.4292 0.3120 0.4196 0.021 Uiso 1 1 calc R
H6B H 0.4677 0.1847 0.2718 0.021 Uiso 1 1 calc R
O1 O 0.53297(14) 0.58886(15) 0.29112(11) 0.0205(2) Uani 1 1 d D
H1 H 0.614(3) 0.554(3) 0.2440(19) 0.031 Uiso 1 1 d D
O2 O 0.46750(16) 0.79324(17) 0.10778(12) 0.0239(2) Uani 1 1 d D
H2E H 0.400(3) 0.693(3) 0.0315(18) 0.036 Uiso 1 1 d D
H2F H 0.485(3) 0.740(3) 0.164(2) 0.036 Uiso 1 1 d D
F F 0.22189(12) 0.49917(13) -0.12899(9) 0.02267(18) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu 0.01087(11) 0.01059(11) 0.01203(11) 0.00386(8) 0.00193(7) 0.00440(8)
N1 0.0148(5) 0.0124(5) 0.0149(5) 0.0049(4) 0.0018(4) 0.0054(4)
N2 0.0135(5) 0.0153(5) 0.0148(5) 0.0052(4) 0.0030(4) 0.0068(4)
C1 0.0178(6) 0.0155(6) 0.0137(6) 0.0067(5) 0.0013(5) 0.0063(5)
C2 0.0190(6) 0.0193(6) 0.0141(6) 0.0073(5) 0.0054(5) 0.0061(5)
C3 0.0151(6) 0.0165(6) 0.0129(6) 0.0034(5) 0.0049(5) 0.0071(5)
C4 0.0172(6) 0.0138(6) 0.0177(6) 0.0034(5) 0.0023(5) 0.0060(5)
C5 0.0129(5) 0.0126(6) 0.0155(6) 0.0026(5) 0.0014(4) 0.0020(5)
C6 0.0143(6) 0.0162(6) 0.0184(6) 0.0037(5) -0.0007(5) 0.0059(5)
O1 0.0147(4) 0.0147(5) 0.0240(5) 0.0038(4) 0.0035(4) 0.0006(4)
O2 0.0210(5) 0.0186(5) 0.0312(6) 0.0104(4) 0.0027(4) 0.0067(4)
F 0.0177(4) 0.0177(4) 0.0325(4) 0.0102(3) 0.0054(3) 0.0063(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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'
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'
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
N2 Cu N2 180.00(6) . 2
N2 Cu N1 88.92(4) . 2
N2 Cu N1 91.08(4) 2 2
N2 Cu N1 91.08(4) . .
N2 Cu N1 88.92(4) 2 .
N1 Cu N1 180.00(5) 2 .
C1 N1 Cu 120.39(8) . .
C3 N2 Cu 120.50(8) . .
N1 C1 C2 110.86(10) . .
N1 C1 C6 110.37(10) . .
C2 C1 C6 110.97(10) . .
C3 C2 C1 112.56(10) . .
N2 C3 C2 110.90(10) . .
N2 C3 C4 109.86(10) . .
C2 C3 C4 111.54(10) . .
C5 C4 C3 112.99(10) . .
O1 C5 C4 107.58(10) . .
O1 C5 C6 111.18(10) . .
C4 C5 C6 110.82(10) . .
C5 C6 C1 113.10(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N2 2.0182(10) .
Cu N2 2.0182(10) 2
Cu N1 2.0200(10) 2
Cu N1 2.0200(10) .
N1 C1 1.4918(16) .
N2 C3 1.4881(16) .
C1 C2 1.5262(17) .
C1 C6 1.5276(17) .
C2 C3 1.5216(18) .
C3 C4 1.5305(17) .
C4 C5 1.5237(17) .
C5 O1 1.4286(15) .
C5 C6 1.5247(18) .
