#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:06:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179313 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/10/4321098.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_4321098
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            'C7 H10 Cl Cu N3 O7'
_chemical_formula_weight         347.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 95.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.606(3)
_cell_length_b                   7.704(2)
_cell_length_c                   21.836(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      12.5
_cell_volume                     2444.6(9)
_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  0.0025
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8850
_diffrn_reflns_theta_max         32.52
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        3.7
_diffrn_standards_interval_time  7200
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    2.039
_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    1.887
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.536
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.936
_refine_ls_goodness_of_fit_obs   0.900
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_restrained_S_obs      0.900
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_obs          0.0472
_refine_ls_shift/esd_max         -1.272
_refine_ls_shift/esd_mean        0.146
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0903P)²+4.7896P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1597
_refine_ls_wR_factor_obs         0.1217
_reflns_number_observed          3164
_reflns_number_total             4425
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991209k_1.cif
_cod_data_source_block           complex1{[Cu(L1)(H2O)](ClO4)}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^)+(0.0903P)^2^+4.7896P] 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^)+(0.0903P)^2^+4.7896P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321098
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.73373(2) 0.52823(5) 0.18253(2) 0.03978(12) Uani 1 d . .
N1 N 0.7395(2) 0.7326(3) 0.12743(12) 0.0440(5) Uani 1 d . .
C2 C 0.6782(2) 0.7181(4) 0.07876(13) 0.0413(5) Uani 1 d . .
N3 N 0.6799(2) 0.8554(4) 0.04187(13) 0.0519(6) Uani 1 d . .
H3A H 0.6456(2) 0.8720(4) 0.00800(13) 0.062 Uiso 1 calc R .
C4 C 0.7467(3) 0.9658(5) 0.0680(2) 0.0590(9) Uani 1 d . .
H4A H 0.7640(3) 1.0720(5) 0.0524(2) 0.071 Uiso 1 calc R .
C5 C 0.7828(3) 0.8886(4) 0.1214(2) 0.0557(8) Uani 1 d . .
H5A H 0.8292(3) 0.9343(4) 0.1490(2) 0.067 Uiso 1 calc R .
C6 C 0.6198(2) 0.5642(4) 0.07315(13) 0.0420(6) Uani 1 d . .
H6A H 0.5757(2) 0.5459(4) 0.04001(13) 0.050 Uiso 1 calc R .
N7 N 0.6343(2) 0.4568(3) 0.11759(10) 0.0365(4) Uani 1 d . .
C8 C 0.5833(2) 0.2946(4) 0.11904(13) 0.0442(6) Uani 1 d . .
H8A H 0.6174(2) 0.2026(4) 0.10116(13) 0.053 Uiso 1 calc R .
H8B H 0.5244(2) 0.3065(4) 0.09455(13) 0.053 Uiso 1 calc R .
C9 C 0.5675(2) 0.2462(4) 0.18476(13) 0.0431(6) Uani 1 d . .
H9A H 0.5350(2) 0.3403(4) 0.20260(13) 0.052 Uiso 1 calc R .
H9B H 0.5286(2) 0.1441(4) 0.18384(13) 0.052 Uiso 1 calc R .
C10 C 0.6556(2) 0.2098(4) 0.22571(12) 0.0381(5) Uani 1 d . .
O11 O 0.72432(14) 0.3092(3) 0.22532(11) 0.0494(5) Uani 1 d . .
O12 O 0.65703(15) 0.0799(3) 0.26069(11) 0.0480(5) Uani 1 d . .
O1W O 0.6031(2) 0.6517(5) 0.2370(2) 0.0801(9) Uani 1 d . .
H1WA H 0.6503(2) 0.5800(5) 0.2588(2) 0.096 Uiso 1 d R .
H1WB H 0.5947(2) 0.7654(5) 0.2547(2) 0.096 Uiso 1 d R .
Cl1 Cl 0.58508(6) 0.14080(11) 0.91564(4) 0.0505(2) Uani 1 d . .
O1A O 0.6564(17) 0.1794(23) 0.8772(6) 0.069(4) Uani 0.44(7) d P 1
O2A O 0.5746(12) 0.2559(21) 0.9635(8) 0.109(4) Uani 0.65(7) d P 1
O3A O 0.5015(13) 0.1656(30) 0.8775(15) 0.104(6) Uani 0.46(7) d P 1
O4A O 0.5923(27) -0.0455(38) 0.9271(11) 0.067(7) Uani 0.47(10) d P 1
O1B O 0.6751(14) 0.1455(37) 0.9007(30) 0.119(12) Uani 0.56(7) d P 2
O2B O 0.5977(37) 0.2361(36) 0.9709(8) 0.088(9) Uani 0.35(7) d P 2
O3B O 0.5214(27) 0.1878(36) 0.8669(9) 0.140(9) Uani 0.54(7) d P 2
O4B O 0.5588(38) -0.0260(41) 0.9355(14) 0.097(8) Uani 0.53(10) 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
O11 Cu1 O12 87.98(10) . 4_655 ?
O11 Cu1 N1 171.61(10) . . ?
O12 Cu1 N1 98.07(11) 4_655 . ?
O11 Cu1 N7 91.19(9) . . ?
O12 Cu1 N7 171.88(9) 4_655 . ?
N1 Cu1 N7 82.00(10) . . ?
O11 Cu1 O1W 90.41(12) . . ?
O12 Cu1 O1W 103.31(10) 4_655 . ?
N1 Cu1 O1W 93.83(12) . . ?
N7 Cu1 O1W 84.77(10) . . ?
C2 N1 C5 106.2(3) . . ?
C2 N1 Cu1 110.6(2) . . ?
C5 N1 Cu1 143.2(2) . . ?
N1 C2 N3 111.5(3) . . ?
N1 C2 C6 118.6(3) . . ?
N3 C2 C6 129.9(3) . . ?
C2 N3 C4 107.3(3) . . ?
C5 C4 N3 106.3(3) . . ?
C4 C5 N1 108.8(3) . . ?
N7 C6 C2 114.3(3) . . ?
C6 N7 C8 121.8(2) . . ?
C6 N7 Cu1 114.4(2) . . ?
C8 N7 Cu1 123.8(2) . . ?
N7 C8 C9 110.9(2) . . ?
C10 C9 C8 113.7(2) . . ?
O12 C10 O11 121.4(2) . . ?
O12 C10 C9 117.8(2) . . ?
O11 C10 C9 120.7(2) . . ?
C10 O11 Cu1 128.7(2) . . ?
C10 O12 Cu1 120.6(2) . 4_645 ?
O4B Cl1 O3B 106.8(20) . . ?
O4B Cl1 O1B 112.8(32) . . ?
O3B Cl1 O1B 113.0(34) . . ?
O4B Cl1 O2B 103.0(17) . . ?
O3B Cl1 O2B 122.7(24) . . ?
O1B Cl1 O2B 98.2(27) . . ?
O2A Cl1 O1A 116.7(9) . . ?
O2A Cl1 O3A 101.7(13) . . ?
O1A Cl1 O3A 105.1(16) . . ?
O2A Cl1 O4A 120.6(11) . . ?
O1A Cl1 O4A 105.1(15) . . ?
O3A Cl1 O4A 106.0(19) . . ?
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 O11 1.940(2) . ?
Cu1 O12 1.961(2) 4_655 ?
Cu1 N1 1.988(3) . ?
Cu1 N7 2.002(2) . ?
Cu1 O1W 2.533(4) . ?
N1 C2 1.324(4) . ?
N1 C5 1.371(4) . ?
C2 N3 1.332(4) . ?
C2 C6 1.459(4) . ?
N3 C4 1.374(5) . ?
C4 C5 1.367(6) . ?
C6 N7 1.276(4) . ?
N7 C8 1.457(4) . ?
C8 C9 1.522(4) . ?
C9 C10 1.517(4) . ?
C10 O12 1.258(3) . ?
C10 O11 1.263(3) . ?
O12 Cu1 1.961(2) 4_645 ?
Cl1 O4B 1.422(14) . ?
Cl1 O3B 1.390(15) . ?
Cl1 O1B 1.386(13) . ?
Cl1 O2A 1.391(14) . ?
Cl1 O2B 1.41(2) . ?
Cl1 O1A 1.43(2) . ?
Cl1 O3A 1.42(2) . ?
Cl1 O4A 1.46(3) . ?
