#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:06:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179313 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/10/4321099.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_4321099
loop_
_publ_author_name
'Enrique Colacio'
'Mustapha Ghazi'
'Raikko Kivekäs'
'José María Moreno'
_publ_contact_author
;
     J.M. Moreno
     Departamento de Química Inorgánica.
     Facultad de Ciencias.
     Universidad de Granada
     18071-Granada
     SPAIN
;
_publ_contact_author_email       jmoreno@ugr.es
_publ_contact_author_fax         +34-958-248526
_publ_contact_author_phone       +34-958-243236
_publ_section_title
;
 Helical-Chain Copper(II) Complexes and a Cyclic Tetranuclear Copper(II)
 Complex with Single Syn-Anti Carboxylate Bridges and Ferromagnetic
 Exchange Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2882
_journal_page_last               2890
_journal_paper_doi               10.1021/ic991209k
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C9 H15 Cl Cu N2 O9'
_chemical_formula_weight         394.22
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.954(3)
_cell_length_b                   7.4866(15)
_cell_length_c                   16.085(3)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.1
_cell_measurement_theta_min      12.7
_cell_volume                     1528.5(6)
_computing_cell_refinement       'STADI4 (STOE, 1995)'
_computing_data_collection       'STADI4 (STOE, 1995)'
_computing_data_reduction        'X-RED  (STOE, 1995)'
_computing_molecular_graphics    'SHELXTL-PC V5.0 (Siemens, 1994)'
_computing_publication_material  'SHELXTL-PC V5.0 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE-Siemens STADI4-4-circle'
_diffrn_measurement_method       ω--2θ
_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  0.0030
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11034
_diffrn_reflns_theta_max         32.49
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        6.0
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_T_max  293(2)
_exptl_absorpt_correction_T_min  293(2)
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Greenish-blue
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.123
_refine_ls_goodness_of_fit_obs   1.131
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         5451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_restrained_S_obs      1.131
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_obs          0.0641
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0441P)²+2.8396P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1588
_refine_ls_wR_factor_obs         0.1211
_reflns_number_observed          3436
_reflns_number_total             5517
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991209k_2.cif
_cod_data_source_block           complex2{[Cu(L2)(H2O)](ClO4).2H2O}n
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+2.8396P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+2.8396P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1528.6(5)
_cod_database_code               4321099
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu1 Cu 0.12953(3) 0.18668(6) 0.31557(3) 0.03497(13) Uani 1 d . .
N1 N 0.2289(2) 0.3779(4) 0.3707(2) 0.0381(7) Uani 1 d . .
C2 C 0.3276(3) 0.3538(5) 0.3578(2) 0.0390(8) Uani 1 d . .
C3 C 0.4086(3) 0.4721(6) 0.3880(3) 0.0510(10) Uani 1 d . .
H3A H 0.4758(3) 0.4540(6) 0.3773(3) 0.061 Uiso 1 calc R .
C4 C 0.3868(4) 0.6185(6) 0.4346(3) 0.0554(11) Uani 1 d . .
H4A H 0.4389(4) 0.7019(6) 0.4549(3) 0.066 Uiso 1 calc R .
C5 C 0.2885(4) 0.6380(6) 0.4502(3) 0.0574(11) Uani 1 d . .
H5A H 0.2735(4) 0.7330(6) 0.4832(3) 0.069 Uiso 1 calc R .
C6 C 0.2098(3) 0.5164(6) 0.4171(3) 0.0496(10) Uani 1 d . .
H6A H 0.1424(3) 0.5324(6) 0.4276(3) 0.059 Uiso 1 calc R .
C7 C 0.3404(3) 0.1916(6) 0.3092(2) 0.0415(8) Uani 1 d . .
H7A H 0.4050(3) 0.1619(6) 0.2960(2) 0.050 Uiso 1 calc R .
N8 N 0.2600(2) 0.0943(4) 0.2861(2) 0.0362(6) Uani 1 d . .
C9 C 0.2640(3) -0.0697(6) 0.2370(3) 0.0459(9) Uani 1 d . .
H9A H 0.2654(3) -0.1727(6) 0.2738(3) 0.055 Uiso 1 calc R .
H9B H 0.3279(3) -0.0707(6) 0.2142(3) 0.055 Uiso 1 calc R .
C10 C -0.1684(3) 0.4184(6) 0.3356(2) 0.0394(8) Uani 1 d . .
H10B H -0.1652(3) 0.5254(6) 0.3700(2) 0.047 Uiso 1 calc R .
H10A H -0.1774(3) 0.3173(6) 0.3713(2) 0.047 Uiso 1 calc R .
C11 C -0.0648(3) 0.3977(5) 0.3063(2) 0.0337(7) Uani 1 d . .
O12 O 0.0439(2) -0.0061(4) 0.2526(2) 0.0436(6) Uani 1 d . .
O13 O -0.0016(2) 0.2824(4) 0.3439(2) 0.0406(6) Uani 1 d . .
O1W O 0.1509(3) 0.0487(5) 0.4464(2) 0.0615(9) Uani 1 d . .
H1WA H 0.1118(3) -0.0515(5) 0.4416(2) 0.092 Uiso 1 d R .
H1WB H 0.2152(3) -0.0014(5) 0.4537(2) 0.092 Uiso 1 d R .
O2W O 0.02824(8) -0.2413(2) 0.47817(7) 0.0635(9) Uani 1 d . .
H2WA H -0.01067(8) -0.2376(2) 0.51865(7) 0.095 Uiso 1 d R .
H2WB H -0.01385(8) -0.1978(2) 0.43117(7) 0.095 Uiso 1 d R .
O3W O 0.11150(8) 0.3614(2) 0.16970(7) 0.0610(9) Uani 1 d R .
H3WA H 0.07585(8) 0.4426(2) 0.19409(7) 0.091 Uiso 1 d R .
H3WB H 0.12565(8) 0.4003(2) 0.12023(7) 0.091 Uiso 1 d R .
Cl1 Cl 0.38276(8) 0.4362(2) 0.12000(7) 0.0683(4) Uani 1 d R .
O21A O 0.33345(8) 0.2563(2) 0.09309(7) 0.152(7) Uani 0.57(2) d PR 1
O22 O 0.30688(8) 0.5226(2) 0.15532(7) 0.140(2) Uani 1 d R 1
O23 O 0.46655(8) 0.3793(2) 0.18197(7) 0.111(2) Uani 1 d R 1
O24A O 0.42911(8) 0.5949(2) 0.08662(7) 0.163(10) Uani 0.50(2) d PR 1
O21B O 0.34161(8) 0.3461(2) 0.06009(7) 0.221(17) Uani 0.43(2) d PR 2
O24B O 0.40477(8) 0.4853(2) 0.04380(7) 0.155(9) Uani 0.50(2) d PR 2
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'
Cl Cl 0.1484 0.1585 '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
N8 Cu1 O12 92.36(12) . . ?
N8 Cu1 O13 179.13(12) . . ?
O12 Cu1 O13 87.84(11) . . ?
N8 Cu1 N1 81.45(13) . . ?
O12 Cu1 N1 173.23(11) . . ?
O13 Cu1 N1 98.30(12) . . ?
N8 Cu1 O1W 96.30(13) . . ?
O12 Cu1 O1W 95.33(13) . . ?
O13 Cu1 O1W 84.53(12) . . ?
N1 Cu1 O1W 88.13(13) . . ?
C6 N1 C2 118.6(3) . . ?
C6 N1 Cu1 129.0(3) . . ?
C2 N1 Cu1 112.4(2) . . ?
N1 C2 C3 122.5(4) . . ?
N1 C2 C7 113.8(3) . . ?
C3 C2 C7 123.8(4) . . ?
C2 C3 C4 118.2(4) . . ?
C5 C4 C3 119.1(4) . . ?
C4 C5 C6 120.1(4) . . ?
N1 C6 C5 121.5(4) . . ?
N8 C7 C2 117.3(3) . . ?
C7 N8 C9 121.7(3) . . ?
C7 N8 Cu1 115.0(3) . . ?
C9 N8 Cu1 123.2(2) . . ?
N8 C9 C10 110.6(3) . 2_545 ?
C11 C10 C9 113.6(3) . 2 ?
O13 C11 O12 122.3(3) . 2 ?
O13 C11 C10 116.9(3) . . ?
O12 C11 C10 120.8(3) 2 . ?
C11 O12 Cu1 128.3(2) 2_545 . ?
C11 O13 Cu1 130.1(2) . . ?
O21B Cl1 O24B 64.6 . . ?
O23 Cl1 O22 111.4 . . ?
O23 Cl1 O24A 101.0 . . ?
O22 Cl1 O24A 98.4 . . ?
O23 Cl1 O21A 99.0 . . ?
O22 Cl1 O21A 103.8 . . ?
O24A Cl1 O21A 142.0 . . ?
Cl1 O21B O24B 63.1 . . ?
Cl1 O24B O21B 52.3 . . ?
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 N8 1.970(3) . ?
Cu1 O12 1.972(3) . ?
Cu1 O13 1.979(2) . ?
Cu1 N1 2.009(3) . ?
Cu1 O1W 2.310(3) . ?
N1 C6 1.330(5) . ?
N1 C2 1.348(5) . ?
C2 C3 1.384(5) . ?
C2 C7 1.471(6) . ?
C3 C4 1.389(6) . ?
C4 C5 1.354(7) . ?
C5 C6 1.390(6) . ?
C7 N8 1.265(5) . ?
N8 C9 1.467(5) . ?
C9 C10 1.526(5) 2_545 ?
C10 C11 1.516(5) . ?
C10 C9 1.526(5) 2 ?
C11 O13 1.258(4) . ?
C11 O12 1.263(4) 2 ?
O12 C11 1.263(4) 2_545 ?
Cl1 O21B 1.21 . ?
Cl1 O24B 1.36 . ?
Cl1 O23 1.39 . ?
Cl1 O22 1.39 . ?
Cl1 O24A 1.48 . ?
Cl1 O21A 1.52 . ?
O21B O24B 1.38 . ?
