#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/77/2007733.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2007733
loop_
_publ_author_name
'Ng, Seik Weng'
'Chen, Xiao-Ming'
'Yang, Guang'
_publ_section_title
;
 Metallo-Ligand [CuII(carboxylato)₄]²⁺ Cores:
 Tetrakis(trimethylammonioacetato-O)copper Diperchlorate and its
 1/1 Complex with Sodium Perchlorate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1389
_journal_page_last               1393
_journal_paper_doi               10.1107/S010827019800523X
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         '[Cu Na (C5 H11 N O2)4 (Cl O4)] (Cl O4)2'
_chemical_formula_sum            'C20 H44 Cl3 Cu N4 Na O20'
_chemical_formula_weight         853.47
_chemical_name_common            'Sodium tetrabetainecopper(II) perchlorate'
_chemical_name_systematic
;
Perchlorato-2\kO-bis(μ-trimethylammonioacetato)-1:2κ⁴O-
bis(trimethylammonioacetato)-1κ²O-coppersodium diperchlorate
;
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.626(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6528(8)
_cell_length_b                   25.8490(10)
_cell_length_c                   5.7717(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.75
_cell_measurement_theta_min      12.25
_cell_volume                     1842.06(19)
_computing_cell_refinement       'CELDIM (Enraf Nonius, 1988)'
_computing_data_collection       'CAD-4/PC (Kretschmar, 1994)'
_computing_data_reduction        'XCAD4 (Harms, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.500
_diffrn_measured_fraction_theta_max 0.500
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'ω 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  0.000
_diffrn_reflns_av_sigmaI/netI    0.028
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2845
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   '\y scan (North et al., 1968)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.909
_refine_ls_abs_structure_details 'Flack & Schwarzenbach (1988)'
_refine_ls_abs_structure_Flack   0.14(3)
_refine_ls_extinction_coef       0.005(2)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.466
_refine_ls_hydrogen_treatment    'Riding model, U(H) = 1.5U~eq~(C)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         2845
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.532
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.195
_reflns_number_observed          2501
_reflns_number_total             2845
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            ka1268.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.1P)^2^] 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^)+(0.1P)^2^] 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        1842.1(2)
_cod_original_sg_symbol_H-M      'C m'
_cod_original_formula_sum        'C20 H44 N4 O20 Na Cl3 Cu'
_cod_database_code               2007733
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu1 0.00425(8) 0 -0.00210(10) 0.0315(3) Uani d S 1 . . Cu
Cl1 -0.4204(3) 0 0.1119(6) 0.0617(8) Uani d SD 1 . . Cl
Cl2 0.4525(2) 0.24880(10) 0.2326(3) 0.0561(5) Uani d PD 0.67 B 2 Cl
Cl2a 0.4525(2) 0.24880(10) 0.2326(3) 0.0561(5) Uani d PD 0.33 C 3 Cl
Na1 -0.1371(3) 0 0.4030(6) 0.0334(7) Uani d S 1 . . Na
O5 -0.3229(9) 0 0.268(4) 0.180(10) Uani d SD 1 . . O
O6 -0.386(2) 0 -0.113(3) 0.23(2) Uani d SD 1 . . O
O7 -0.4753(8) 0.0444(3) 0.101(3) 0.137(5) Uani d D 1 . . O
O8 0.3701(2) 0.2755(8) 0.288(4) 0.162(5) Uani d PD 0.67 B 2 O
O9 0.441(2) 0.1942(7) 0.268(4) 0.162(5) Uani d PD 0.67 B 2 O
O10 0.449(2) 0.2551(9) -0.014(3) 0.162(5) Uani d PD 0.67 B 2 O
O11 0.556(2) 0.2606(8) 0.358(4) 0.162(5) Uani d PD 0.67 B 2 O
O8a 0.336(3) 0.259(2) 0.133(7) 0.21(2) Uani d PD 0.33 C 3 O
O9a 0.521(4) 0.283(2) 0.129(7) 0.21(2) Uani d PD 0.33 C 3 O
O10a 0.475(4) 0.1940(10) 0.174(6) 0.21(2) Uani d PD 0.33 C 3 O
O11a 0.475(4) 0.2530(10) 0.493(6) 0.21(2) Uani d PD 0.33 C 3 O
O1a 0.097(2) 0.0584(9) -0.045(3) 0.040(4) Uani d PU 0.50 A -1 O
O2a 0.2600(10) 0.0300(10) 0.157(4) 0.122(9) Uani d PU 0.50 A -1 O
N1a 0.200(2) 0.1341(6) -0.283(3) 0.043(5) Uani d PDU 0.50 A -1 N
C1a 0.2040(10) 0.0585(6) 0.007(3) 0.048(3) Uani d PDU 0.50 A -1 C
C2a 0.2680(10) 0.0954(9) -0.117(4) 0.069(6) Uani d PDU 0.50 A -1 C
C3a 0.121(2) 0.1065(8) -0.477(4) 0.077(6) Uani d PDU 0.50 A -1 C
C4a 0.142(2) 0.1689(8) -0.147(4) 0.077(6) Uani d PDU 0.50 A -1 C
C5a 0.274(2) 0.1672(8) -0.396(4) 0.077(6) Uani d PDU 0.50 A -1 C
O1b 0.093(2) -0.0489(9) -0.129(4) 0.052(5) Uani d PU 0.50 . -1 O
O2b 0.0480(10) -0.0157(4) -0.490(2) 0.050(3) Uani d PU 0.50 . -1 O
N1b 0.2190(10) -0.1257(6) -0.289(3) 0.041(5) Uani d PDU 0.50 . -1 N
C1b 0.0890(10) -0.0477(5) -0.347(2) 0.037(2) Uani d PDU 0.50 . -1 C
C2b 0.1520(10) -0.0873(7) -0.463(3) 0.057(5) Uani d PDU 0.50 . -1 C
C3b 0.306(2) -0.0990(9) -0.104(4) 0.063(4) Uani d PDU 0.50 . -1 C
C4b 0.147(2) -0.1607(8) -0.177(5) 0.063(4) Uani d PDU 0.50 . -1 C
C5b 0.275(2) -0.1597(8) -0.449(4) 0.063(4) Uani d PDU 0.50 . -1 C
O3 -0.0950(4) 0.0517(2) 0.0708(9) 0.0380(10) Uani d . 1 . . O
O4 -0.1531(5) 0.0644(2) -0.3183(9) 0.0480(10) Uani d . 1 . . O
N2 -0.3011(5) 0.1432(2) -0.2340(9) 0.0360(10) Uani d . 1 . . N
C6 -0.1532(5) 0.0734(3) -0.1100(10) 0.0340(10) Uani d . 1 . . C
C7 -0.2296(6) 0.1133(3) -0.0400(10) 0.0360(10) Uani d . 1 . . C
C8 -0.3769(7) 0.1067(4) -0.393(2) 0.059(2) Uani d . 1 . . C
C9 -0.2389(8) 0.1731(3) -0.376(2) 0.053(2) Uani d . 1 . . C
C10 -0.3687(9) 0.1782(4) -0.119(2) 0.062(2) Uani d . 1 . . C
H2a1 0.3194 0.1143 0.0029 0.103 Uiso calc PR 0.50 A -1 H
H2a2 0.3096 0.0751 -0.2073 0.103 Uiso calc PR 0.50 A -1 H
H3a1 0.1603 0.0844 -0.5622 0.116 Uiso calc PR 0.50 A -1 H
H3a2 0.0806 0.1314 -0.5839 0.116 Uiso calc PR 0.50 A -1 H
H3a3 0.0725 0.0860 -0.4084 0.116 Uiso calc PR 0.50 A -1 H
H4a1 0.1937 0.1858 -0.0238 0.116 Uiso calc PR 0.50 A -1 H
H4a2 0.0926 0.1491 -0.0782 0.116 Uiso calc PR 0.50 A -1 H
H4a3 0.1024 0.1945 -0.2522 0.116 Uiso calc PR 0.50 A -1 H
H5a1 0.3118 0.1456 -0.4860 0.116 Uiso calc PR 0.50 A -1 H
H5a2 0.3249 0.1848 -0.2744 0.116 Uiso calc PR 0.50 A -1 H
H5a3 0.2313 0.1922 -0.4998 0.116 Uiso calc PR 0.50 A -1 H
H2b1 0.1004 -0.1064 -0.5817 0.086 Uiso calc PR 0.50 . -1 H
H2b2 0.1995 -0.0688 -0.5444 0.086 Uiso calc PR 0.50 . -1 H
H3b1 0.3487 -0.0772 -0.1813 0.095 Uiso calc PR 0.50 . -1 H
H3b2 0.3512 -0.1247 -0.0109 0.095 Uiso calc PR 0.50 . -1 H
H3b3 0.2720 -0.0784 -0.0017 0.095 Uiso calc PR 0.50 . -1 H
H4b1 0.0927 -0.1761 -0.2998 0.095 Uiso calc PR 0.50 . -1 H
H4b2 0.1132 -0.1407 -0.0739 0.095 Uiso calc PR 0.50 . -1 H
H4b3 0.1907 -0.1874 -0.0876 0.095 Uiso calc PR 0.50 . -1 H
H5b1 0.3214 -0.1384 -0.5204 0.095 Uiso calc PR 0.50 . -1 H
H5b2 0.2214 -0.1757 -0.5705 0.095 Uiso calc PR 0.50 . -1 H
H5b3 0.3178 -0.1859 -0.3535 0.095 Uiso calc PR 0.50 . -1 H
H7a -0.2755 0.0955 0.0484 0.054 Uiso calc R 1 . . H
H7b -0.1860 0.1378 0.0670 0.054 Uiso calc R 1 . . H
H8a -0.4172 0.0873 -0.2993 0.088 Uiso calc R 1 . . H
H8b -0.3359 0.0835 -0.4685 0.088 Uiso calc R 1 . . H
H8c -0.4261 0.1262 -0.5110 0.088 Uiso calc R 1 . . H
H9a -0.2879 0.1917 -0.4977 0.079 Uiso calc R 1 . . H
H9b -0.1958 0.1500 -0.4467 0.079 Uiso calc R 1 . . H
H9c -0.1925 0.1971 -0.2745 0.079 Uiso calc R 1 . . H
H10a -0.4086 0.1579 -0.0281 0.093 Uiso calc R 1 . . H
H10b -0.4183 0.1970 -0.2395 0.093 Uiso calc R 1 . . H
H10c -0.3226 0.2021 -0.0166 0.093 Uiso calc R 1 . . H
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'
Na Na 0.0362 0.0249 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1a Cu1 O1b . . 92.4(6) yes
O1a Cu1 O3 . . 86.1(6) yes
O1a Cu1 O3 . 2 172.2(5) yes
O1b Cu1 O3 . . 170.5(6) yes
O1b Cu1 O3 . 2 95.0(7) yes
O3 Cu1 O3 . 2 87.0(3) yes
O2b Na1 O3 2_556 . 74.8(3) yes
O2b Na1 O3 2_556 2 85.7(3) yes
O2b Na1 O4 2_556 1_556 85.9(3) yes
O2b Na1 O4 2_556 2_556 100.1(3) yes
O2b Na1 O5 2_556 . 169.2(3) yes
O3 Na1 O3 . 2 65.0(3) yes
O3 Na1 O4 . 1_556 102.2(2) yes
O3 Na1 O4 . 2_556 166.2(2) yes
O3 Na1 O5 . . 96.5(5) yes
O3 Na1 O4 2 1_556 166.2(2) yes
O3 Na1 O4 2 2_556 102.2(2) yes
O3 Na1 O5 2 . 96.5(5) yes
O4 Na1 O4 1_556 2_556 90.0(3) yes
O4 Na1 O5 1_556 . 89.8(5) yes
O4 Na1 O5 2_556 . 89.8(5) yes
C1a O1a Cu1 . . 126(2) ?
C4a N1a C3a . . 111.0(10) ?
C4a N1a C2a . . 110.0(10) ?
C3A N1a C2a . . 111.0(10) ?
C4a N1a C5a . . 108.0(10) ?
C3a N1a C5a . . 109.0(10) ?
C2a N1a C5a . . 109.0(10) ?
O2a C1a O1a . . 124(2) ?
O2a C1a C2a . . 115.0(10) ?
O1a C1a C2a . . 121(2) ?
N1a C2a C1a . . 115.0(10) ?
C1b O1b Cu1 . . 118(2) ?
C1b O2b Na1 . 1_554 124.0(10) ?
C4b N1b C3b . . 112.0(10) ?
C4b N1b C2b . . 111.0(10) ?
C3b N1b C2b . . 112.0(10) ?
C4b N1b C5b . . 108.0(10) ?
C3b N1b C5b . . 109.0(10) ?
C2b N1b C5b . . 104.0(10) ?
O2b C1b O1b . . 129(2) ?
O2b C1b C2b . . 110.0(10) ?
O1b C1b C2b . . 121(2) ?
N1b C2b C1b . . 114.0(10) ?
C6 O3 Cu1 . . 114.3(4) ?
C6 O3 Na1 . . 133.5(4) ?
Cu1 O3 Na1 . . 93.1(2) ?
C6 O4 Na1 . 1_554 145.5(5) ?
C9 N2 C7 . . 112.2(6) ?
C9 N2 C10 . . 110.8(6) ?
C7 N2 C10 . . 107.1(5) ?
C9 N2 C8 . . 109.8(6) ?
C7 N2 C8 . . 109.5(6) ?
C10 N2 C8 . . 107.3(7) ?
O3 C6 O4 . . 126.8(7) ?
O4 C6 C7 . . 121.7(6) ?
O3 C6 C7 . . 111.5(5) ?
N2 C7 C6 . . 117.8(5) ?
O5 Cl1 O6 . . 101.0(10) ?
O5 Cl1 O7 . . 114.8(6) ?
O5 Cl1 O7 . 2 114.8(6) ?
O6 Cl1 O7 . . 102.2(7) ?
O6 Cl1 O7 . 2 102.2(7) ?
O7 Cl1 O7 . 2 118.3(9) ?
Cl1 O5 Na1 . . 159(2) ?
O8 Cl2 O9 . . 111.0(10) ?
O8 Cl2 O10 . . 109.0(10) ?
O9 Cl2 O10 . . 106.0(10) ?
O8 Cl2 O11 . . 117.0(10) ?
O9 Cl2 O11 . . 105.0(10) ?
O10 Cl2 O11 . . 108.0(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 O1a . 1.96(2) yes
Cu1 O1b . 1.94(2) yes
Cu1 O3 . 1.942(5) yes
Cu1 O3 2 1.942(5) yes
Cu1 Na1 . 3.239(3) no
Cu1 Na1 1_554 3.508(3) no
Na1 O2b 2_556 2.330(10) yes
Na1 O3 . 2.489(6) yes
Na1 O3 2 2.489(6) yes
Na1 O4 1_556 2.354(5) yes
Na1 O4 2_556 2.354(5) yes
Na1 O5 . 2.310(10) yes
O1a C1a . 1.32(3) ?
O2a C1a . 1.24(2) ?
N1a C4a . 1.49(2) ?
N1a C3a . 1.50(2) ?
N1a C2a . 1.520(10) ?
N1a C5a . 1.52(2) ?
C1a C2a . 1.530(10) ?
O1b C1b . 1.25(2) ?
O2b C1b . 1.21(2) ?
N1b C4b . 1.52(2) ?
N1b C3b . 1.52(2) ?
N1b C2b . 1.530(10) ?
N1b C5b . 1.55(2) ?
C1b C2b . 1.530(10) ?
O3 C6 . 1.270(9) ?
O4 C6 . 1.223(8) ?
N2 C7 . 1.491(8) ?
N2 C8 . 1.504(9) ?
N2 C9 . 1.471(9) ?
N2 C10 . 1.496(9) ?
C6 C7 . 1.527(9) ?
Cl1 O5 . 1.360(10) ?
Cl1 O6 . 1.460(10) ?
Cl1 O7 . 1.340(10) ?
Cl1 O7 2 1.340(10) ?
Cl2 O8 . 1.34(2) ?
Cl2 O9 . 1.44(2) ?
Cl2 O10 . 1.42(2) ?
Cl2 O11 . 1.39(2) ?
