#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:08:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179314 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/11/4321100.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_4321100
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            'C10 H17 Cl Cu N2 O9'
_chemical_formula_weight         408.25
_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                 100.432(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1234(10)
_cell_length_b                   7.7098(4)
_cell_length_c                   16.126(2)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.46
_cell_measurement_theta_min      6.86
_cell_volume                     1604.6(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'SHELXTL-PC V5.0 (Siemens, 1994)'
_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       'Siemens P4'
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5048
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        1.9
_diffrn_standards_interval_count 90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.574
_exptl_absorpt_correction_T_max  293(2)
_exptl_absorpt_correction_T_min  293(2)
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.034
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.192
_refine_ls_restrained_S_obs      1.034
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_obs          0.0429
_refine_ls_shift/esd_max         4.287
_refine_ls_shift/esd_mean        0.321
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0520P)²+1.4314P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1404
_refine_ls_wR_factor_obs         0.1067
_reflns_number_observed          3178
_reflns_number_total             4119
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991209k_3.cif
_cod_data_source_block           complex3{[Cu(L3)(H2O)](ClO4)}n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+1.4314P] 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^)+(0.0520P)^2^+1.4314P] 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        1604.6(2)
_cod_database_code               4321100
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 0.37741(2) 0.29349(5) 0.19111(2) 0.04074(12) Uani 1 d . .
N1 N 0.2797(2) 0.1157(3) 0.1306(2) 0.0460(6) Uani 1 d . .
C2 C 0.1818(2) 0.1406(5) 0.1434(2) 0.0506(7) Uani 1 d . .
C3 C 0.1015(3) 0.0328(6) 0.1089(3) 0.0690(11) Uani 1 d . .
H3A H 0.0349(3) 0.0507(6) 0.1194(3) 0.083 Uiso 1 calc R .
C4 C 0.1224(3) -0.1032(6) 0.0582(3) 0.0815(14) Uani 1 d . .
H4A H 0.0701(3) -0.1793(6) 0.0348(3) 0.098 Uiso 1 calc R .
C5 C 0.2211(3) -0.1241(6) 0.0431(3) 0.0745(12) Uani 1 d . .
H5A H 0.2359(3) -0.2125(6) 0.0079(3) 0.089 Uiso 1 calc R .
C6 C 0.2987(3) -0.0124(5) 0.0808(2) 0.0595(9) Uani 1 d . .
H6A H 0.3658(3) -0.0279(5) 0.0709(2) 0.071 Uiso 1 calc R .
C7 C 0.1682(2) 0.2905(5) 0.1958(2) 0.0541(8) Uani 1 d . .
H7A H 0.1040(2) 0.3182(5) 0.2087(2) 0.065 Uiso 1 calc R .
N8 N 0.2482(2) 0.3815(4) 0.2228(2) 0.0473(6) Uani 1 d . .
C9 C 0.2424(2) 0.5383(6) 0.2744(3) 0.0595(9) Uani 1 d . .
H9A H 0.1678(106) 0.5283(185) 0.3118(94) 0.071 Uiso 0.47(3) d P 1
H9B H 0.2383(73) 0.6206(137) 0.2396(63) 0.071 Uiso 0.53(3) d P 2
C10 C 0.6615(2) 0.0491(5) 0.1578(2) 0.0506(7) Uani 1 d . .
H10A H 0.6701(2) 0.1436(5) 0.1199(2) 0.061 Uiso 1 calc R .
H10B H 0.6556(2) -0.0574(5) 0.1252(2) 0.061 Uiso 1 calc R .
C11 C 0.5615(2) 0.0770(4) 0.1908(2) 0.0402(6) Uani 1 d . .
O12 O 0.4625(2) 0.4779(3) 0.25376(14) 0.0475(5) Uani 1 d . .
O13 O 0.5047(2) 0.2001(3) 0.15941(14) 0.0450(5) Uani 1 d . .
C14A C 0.2242(8) 0.6842(10) 0.2237(7) 0.068(3) Uani 0.55(2) d P 1
H14A H 0.1624(8) 0.6673(10) 0.1824(7) 0.102 Uiso 0.52(10) calc PR 1
H14B H 0.2819(8) 0.7031(10) 0.1957(7) 0.102 Uiso 0.87(11) calc PR 1
H14C H 0.2155(8) 0.7833(10) 0.2578(7) 0.102 Uiso 0.66(10) calc PR 1
C14B C 0.1437(8) 0.5799(14) 0.2966(7) 0.060(4) Uiso 0.41(2) d P 2
H14D H 0.0902(8) 0.5689(14) 0.2477(7) 0.090 Uiso 0.70(9) calc PR 2
H14E H 0.1451(8) 0.6968(14) 0.3173(7) 0.090 Uiso 0.51(10) calc PR 2
H14F H 0.1301(8) 0.5017(14) 0.3396(7) 0.090 Uiso 0.64(12) calc PR 2
O1W O 0.3593(2) 0.4475(4) 0.0634(2) 0.0725(8) Uani 1 d . .
H1WA H 0.4040(2) 0.5283(4) 0.0680(2) 0.109 Uiso 1 d R .
H1WB H 0.2987(2) 0.4902(4) 0.0516(2) 0.109 Uiso 1 d R .
O2W O 0.4717(2) 0.7351(4) 0.0231(2) 0.0742(8) Uani 1 d . .
H2WA H 0.5200(2) 0.7722(4) 0.0614(2) 0.111 Uiso 1 d R .
H2WB H 0.4971(2) 0.7037(4) -0.0194(2) 0.111 Uiso 1 d R .
O3W O 0.3924(2) 0.1155(4) 0.3327(2) 0.0675(7) Uani 1 d . .
H3WA H 0.3319(2) 0.0876(4) 0.3396(2) 0.101 Uiso 1 d R .
H3WB H 0.4242(2) 0.0718(4) 0.2962(2) 0.101 Uiso 1 d R .
Cl1 Cl 0.87909(8) 0.5564(2) 0.10125(7) 0.0765(3) Uani 1 d . .
O20 O 0.9445(5) 0.4110(11) 0.0963(6) 0.201(3) Uani 1 d . 1
O21A O 0.9114(28) 0.7196(29) 0.1255(22) 0.222(17) Uani 0.47(3) d P 1
O22A O 0.8639(12) 0.5449(29) 0.0112(8) 0.136(7) Uani 0.48(3) d P 1
O23A O 0.7814(16) 0.4623(37) 0.1044(16) 0.086(9) Uani 0.35(9) d P 1
O21B O 0.9387(12) 0.6013(40) 0.1729(13) 0.222(11) Uani 0.53(3) d P 2
O22B O 0.8448(18) 0.6688(44) 0.0431(23) 0.254(20) Uani 0.52(3) d P 2
O23B O 0.7996(28) 0.5169(57) 0.1393(42) 0.169(13) Uani 0.65(9) d P 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
O13 Cu1 O12 88.20(9) . . ?
O13 Cu1 N8 178.59(10) . . ?
O12 Cu1 N8 93.03(9) . . ?
O13 Cu1 N1 96.98(10) . . ?
O12 Cu1 N1 174.82(9) . . ?
N8 Cu1 N1 81.79(10) . . ?
O13 Cu1 O1W 85.03(10) . . ?
O12 Cu1 O1W 92.46(10) . . ?
N8 Cu1 O1W 95.61(11) . . ?
N1 Cu1 O1W 87.99(11) . . ?
C6 N1 C2 119.1(3) . . ?
C6 N1 Cu1 129.1(2) . . ?
C2 N1 Cu1 111.8(2) . . ?
N1 C2 C3 122.1(3) . . ?
N1 C2 C7 114.8(3) . . ?
C3 C2 C7 123.1(3) . . ?
C2 C3 C4 118.4(3) . . ?
C5 C4 C3 119.2(4) . . ?
C4 C5 C6 119.5(4) . . ?
N1 C6 C5 121.6(3) . . ?
N8 C7 C2 117.1(3) . . ?
C7 N8 C9 121.4(3) . . ?
C7 N8 Cu1 114.5(2) . . ?
C9 N8 Cu1 124.0(2) . . ?
C14A C9 N8 110.7(5) . . ?
C14B C9 N8 117.5(5) . . ?
C14A C9 C10 114.5(5) . 2_655 ?
C14B C9 C10 118.4(5) . 2_655 ?
N8 C9 C10 109.3(3) . 2_655 ?
C11 C10 C9 114.4(3) . 2_645 ?
O13 C11 O12 122.6(2) . 2_645 ?
O13 C11 C10 117.0(2) . . ?
O12 C11 C10 120.4(3) 2_645 . ?
C11 O12 Cu1 127.7(2) 2_655 . ?
C11 O13 Cu1 129.9(2) . . ?
O22B Cl1 O23B 106.6(20) . . ?
O22B Cl1 O21B 122.1(22) . . ?
O23B Cl1 O21B 92.7(36) . . ?
O21A Cl1 O20 125.7(17) . . ?
O21A Cl1 O22A 109.1(16) . . ?
O20 Cl1 O22A 82.5(9) . . ?
O21A Cl1 O23A 132.0(16) . . ?
O20 Cl1 O23A 98.7(12) . . ?
O22A Cl1 O23A 92.4(12) . . ?
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 O13 1.970(2) . ?
Cu1 O12 1.970(2) . ?
Cu1 N8 1.978(2) . ?
Cu1 N1 2.006(3) . ?
Cu1 O1W 2.352(3) . ?
N1 C6 1.325(4) . ?
N1 C2 1.352(4) . ?
C2 C3 1.378(5) . ?
C2 C7 1.461(5) . ?
C3 C4 1.387(6) . ?
C4 C5 1.370(6) . ?
C5 C6 1.388(5) . ?
C7 N8 1.271(4) . ?
N8 C9 1.478(4) . ?
C9 C14A 1.386(9) . ?
C9 C14B 1.442(10) . ?
C9 C10 1.514(5) 2_655 ?
C10 C11 1.519(4) . ?
C10 C9 1.514(5) 2_645 ?
C11 O13 1.255(3) . ?
C11 O12 1.259(4) 2_645 ?
O12 C11 1.259(4) 2_655 ?
Cl1 O22B 1.296(11) . ?
Cl1 O23B 1.337(12) . ?
Cl1 O21B 1.318(11) . ?
Cl1 O21A 1.363(13) . ?
Cl1 O20 1.423(7) . ?
Cl1 O22A 1.432(12) . ?
Cl1 O23A 1.48(2) . ?
