#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:06:44 +0100 (mar 08 de nov de 2016) $
#$Revision: 188233 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/08/7040800.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_7040800
loop_
_publ_author_name
'Yoneyama, Shota'
'Kodama, Takeshi'
'Kikuchi, Koichi'
'Fujisawa, Takumi'
'Yamaguchi, Akira'
'Sumiyama, Akihiko'
'Shuku, Yoshiaki'
'Aoyagi, Shinobu'
'Fujita, Wataru'
_publ_section_title
;
 Deuterium substitution effects on the structural and magnetic phase
 transitions of a hydrogen-bonded coordination polymer,
 bis(glycolato)copper(ii).
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16774
_journal_page_last               16778
_journal_paper_doi               10.1039/c6dt03592b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C4 H6 Cu O6'
_chemical_formula_sum            'C4 H6 Cu O6'
_chemical_formula_weight         213.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-09-29 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 106.812(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   5.108(2)
_cell_length_b                   8.677(3)
_cell_length_c                   7.755(3)
_cell_measurement_reflns_used    769
_cell_measurement_temperature    290
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.60
_cell_volume                     329.0(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      290
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2343
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         3.612
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.297
_exptl_absorpt_correction_T_max  0.517
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, ????)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             214.00
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     56
_refine_ls_number_reflns         747
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0362P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                627
_reflns_number_total             748
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c6dt03592b2.cif
_cod_data_source_block           13093001
_cod_depositor_comments
'Adding full bibliography for 7040794--7040800.cif.'
_cod_database_code               7040800
_shelx_res_file
;

    shelxl.res created by SHELXL-2014/7

TITL 13093001
CELL  0.71075 5.10800 8.67700 7.75500 90.00000 106.81200 90.00000
ZERR  2 0.00200 0.00300 0.00300 0.00000 0.00400 0.00000
LATT 1
SYMM .50-X, .50+Y, .50-Z
SFAC C H CU O
UNIT 8 12 2 12
L.S. 20
FMAP 2
PLAN 25
WPDB -2
HTAB
BOND $H
CONF
LIST 4
TEMP -100.0
ACTA
SIZE 0.200 0.200 0.700
WGHT    0.036200
FVAR       3.93371
CU1   3    0.500000    0.500000    0.500000    10.50000    0.02917    0.01858 =
         0.03066   -0.00347    0.02132   -0.00320
O2    4    0.547197    0.339120    0.341770    11.00000    0.03241    0.02265 =
         0.03373   -0.00533    0.02384   -0.00476
O3    4    0.258023    0.352356    0.562216    11.00000    0.03491    0.02535 =
         0.03433   -0.00633    0.02746   -0.00598
O4    4    0.409605    0.104839    0.241613    11.00000    0.03339    0.02772 =
         0.03382   -0.01137    0.02082   -0.00654
C5    1    0.407336    0.217954    0.340566    11.00000    0.01948    0.02535 =
         0.02048    0.00066    0.00863    0.00246
C6    1    0.231865    0.210175    0.467827    11.00000    0.03106    0.02648 =
         0.03174   -0.00797    0.02054   -0.00799
AFIX  23
H6A   2    0.038358    0.192391    0.399110    11.00000   -1.20000
H6B   2    0.292828    0.124115    0.553922    11.00000   -1.20000
AFIX   0
H3    2    0.161338    0.364050    0.610969    11.00000    0.03846
HKLF 4

REM  13093001
REM R1 =  0.0265 for     627 Fo > 4sig(Fo)  and  0.0312 for all     747 data
REM     56 parameters refined using      0 restraints

END

WGHT      0.0359      0.0000

REM Instructions for potential hydrogen bonds
EQIV $1 x-1/2, -y+1/2, z-1/2
HTAB C6 O3_$1
EQIV $2 x-1/2, -y+1/2, z+1/2
HTAB O3 O4_$2

REM Highest difference peak  0.295,  deepest hole -0.646,  1-sigma level  0.105
Q1    1  -0.1744  0.1436  0.4114  11.00000  0.05    0.29
Q2    1   0.3479  0.2043  0.4159  11.00000  0.05    0.28
Q3    1   0.0243  0.1015  0.4464  11.00000  0.05    0.28
Q4    1   0.3449  0.0573  0.2439  11.00000  0.05    0.28
Q5    1   0.6271  0.0826  0.4285  11.00000  0.05    0.25
Q6    1  -0.0965  0.0757  0.3372  11.00000  0.05    0.23
Q7    1  -0.0427  0.2388  0.2964  11.00000  0.05    0.22
Q8    1  -0.0250 -0.0011  0.3739  11.00000  0.05    0.22
Q9    1   0.5327  0.4857  0.2428  11.00000  0.05    0.21
Q10   1  -0.2153  0.2708  0.2930  11.00000  0.05    0.20
Q11   1   0.4143  0.1136  0.5956  11.00000  0.05    0.20
Q12   1   0.7561  0.2203  0.5305  11.00000  0.05    0.20
Q13   1   0.0756  0.2547  0.2858  11.00000  0.05    0.19
Q14   1   0.2904 -0.0041  0.5915  11.00000  0.05    0.18
Q15   1   0.4673  0.3232  0.6869  11.00000  0.05    0.18
Q16   1   0.7939  0.3419  0.4568  11.00000  0.05    0.18
Q17   1   0.6038  0.3432  0.3004  11.00000  0.05    0.18
Q18   1   0.2543 -0.0034  0.1477  11.00000  0.05    0.17
Q19   1   0.1658 -0.0773  0.4737  11.00000  0.05    0.17
Q20   1   0.5479  0.2715  0.3615  11.00000  0.05    0.16
Q21   1  -0.0052  0.1543  0.5217  11.00000  0.05    0.16
Q22   1   0.5132 -0.0011  0.3669  11.00000  0.05    0.15
Q23   1   0.5161  0.2162  0.6422  11.00000  0.05    0.15
Q24   1   0.5032  0.4050  0.3625  11.00000  0.05    0.15
Q25   1   0.0668  0.0607  0.2370  11.00000  0.05    0.15
;
_shelx_res_checksum              93818
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5000 0.5000 0.5000 0.02347(17) Uani 1 2 d S . P
O2 O 0.5472(4) 0.3391(2) 0.3418(3) 0.0266(4) Uani 1 1 d . . .
O3 O 0.2580(4) 0.3524(2) 0.5622(3) 0.0279(5) Uani 1 1 d . . .
O4 O 0.4096(4) 0.10484(19) 0.2416(3) 0.0293(4) Uani 1 1 d . . .
C5 C 0.4073(5) 0.2180(3) 0.3406(3) 0.0212(5) Uani 1 1 d . . .
C6 C 0.2319(6) 0.2102(3) 0.4678(4) 0.0274(6) Uani 1 1 d . . .
H6A H 0.0384 0.1924 0.3991 0.033 Uiso 1 1 calc R U .
H6B H 0.2928 0.1241 0.5539 0.033 Uiso 1 1 calc R U .
H3 H 0.161(7) 0.364(3) 0.611(4) 0.038(10) Uiso 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
Cu1 0.0292(3) 0.0186(3) 0.0307(3) -0.00347(18) 0.0213(2) -0.00320(17)
O2 0.0324(10) 0.0227(9) 0.0337(11) -0.0053(8) 0.0238(9) -0.0048(8)
O3 0.0349(11) 0.0254(10) 0.0343(11) -0.0063(8) 0.0275(10) -0.0060(8)
O4 0.0334(10) 0.0277(10) 0.0338(11) -0.0114(8) 0.0208(9) -0.0065(8)
C5 0.0195(12) 0.0253(13) 0.0205(13) 0.0007(10) 0.0086(10) 0.0025(10)
C6 0.0311(14) 0.0265(13) 0.0317(15) -0.0080(11) 0.0205(12) -0.0080(11)
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(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
O2 Cu1 O2 180.00(10) . 3_666
O2 Cu1 O3 83.42(8) . .
O2 Cu1 O3 96.58(8) 3_666 .
O2 Cu1 O3 96.59(8) . 3_666
O2 Cu1 O3 83.42(8) 3_666 3_666
O3 Cu1 O3 180.0 . 3_666
C5 O2 Cu1 115.63(15) . .
C6 O3 Cu1 114.70(15) . .
C6 O3 H3 115(3) . .
Cu1 O3 H3 129(2) . .
O4 C5 O2 123.4(2) . .
O4 C5 C6 118.6(2) . .
O2 C5 C6 118.0(2) . .
O3 C6 C5 108.17(19) . .
O3 C6 H6A 110.1 . .
C5 C6 H6A 110.1 . .
O3 C6 H6B 110.1 . .
C5 C6 H6B 110.1 . .
H6A C6 H6B 108.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.9193(17) .
Cu1 O2 1.9193(17) 3_666
Cu1 O3 1.9356(18) .
Cu1 O3 1.9357(18) 3_666
O2 C5 1.270(3) .
O3 C6 1.421(3) .
O3 H3 0.71(3) .
O4 C5 1.248(3) .
C5 C6 1.514(3) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O3 H3 O4 4_566 2.583(3) 0.71(4) 1.87(4) 179(3) no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Cu1 O2 C5 O4 178.03(19)
Cu1 O2 C5 C6 -2.8(3)
Cu1 O3 C6 C5 -0.4(3)
O4 C5 C6 O3 -178.7(2)
O2 C5 C6 O3 2.1(3)
