#------------------------------------------------------------------------------
#$Date: 2019-11-24 05:17:52 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236814 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/70/7237087.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_7237087
loop_
_publ_author_name
'Pasán, Jorge'
'Sanchiz, Joaquín'
'Lloret, Francesc'
'Julve, Miguel'
'Ruiz-Pérez, Catalina'
_publ_section_title
;
 Magnetostructural relationships in polymorphic ethylmalonate-containing
 copper(ii) coordination polymers
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              7464
_journal_paper_doi               10.1039/C8CE01595C
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_sum            'C10 H22 Cu2 O13'
_chemical_formula_weight         477.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-09-12 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9885(2)
_cell_length_b                   11.9939(2)
_cell_length_c                   14.1518(3)
_cell_measurement_reflns_used    8647
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.6240
_cell_measurement_theta_min      2.8540
_cell_volume                     1695.40(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13228
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.882
_diffrn_reflns_theta_min         2.654
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.321
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.211
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.005(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2801
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0213P)²+0.8872P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0494
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                2706
_reflns_number_total             2801
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce01595c2.cif
_cod_data_source_block           compound1
_cod_database_code               7237087
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+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
C1 C 0.2641(2) 0.44717(16) 0.71787(15) 0.0162(4) Uani 1 1 d . . .
C2 C 0.2601(2) 0.46064(17) 0.82497(15) 0.0186(4) Uani 1 1 d . . .
H2 H 0.169(3) 0.4898(9) 0.8427(5) 0.022 Uiso 1 1 calc R U .
C3 C 0.2818(2) 0.35097(18) 0.87736(14) 0.0183(4) Uani 1 1 d . . .
C4 C 0.3647(3) 0.54648(19) 0.85801(17) 0.0269(5) Uani 1 1 d . . .
H4A H 0.3642(3) 0.5491(2) 0.9264(15) 0.032 Uiso 1 1 calc R U .
H4B H 0.453(2) 0.5217(6) 0.8382(5) 0.032 Uiso 1 1 calc R U .
C5 C 0.3412(4) 0.6631(2) 0.8202(3) 0.0459(8) Uani 1 1 d . . .
H5A H 0.345(3) 0.6620(5) 0.7538(16) 0.069 Uiso 1 1 calc R U .
H5B H 0.408(2) 0.7114(12) 0.8437(16) 0.069 Uiso 1 1 calc R U .
H5C H 0.256(2) 0.6884(11) 0.8397(16) 0.069 Uiso 1 1 calc R U .
Cu1 Cu 0.5000 0.30127(3) 0.7500 0.01738(8) Uani 1 2 d S T P
Cu2 Cu 0.17474(4) 0.5000 0.5000 0.01816(8) Uani 1 2 d S T P
O1 O 0.17624(17) 0.49325(16) 0.66904(10) 0.0245(3) Uani 1 1 d . . .
O2 O 0.35978(16) 0.39171(14) 0.68127(11) 0.0204(3) Uani 1 1 d . . .
O3 O 0.19825(18) 0.32308(16) 0.93742(14) 0.0343(5) Uani 1 1 d . . .
O4 O 0.38650(16) 0.29278(14) 0.86168(10) 0.0212(3) Uani 1 1 d . . .
O1W O 0.5000 0.13456(18) 0.7500 0.0324(6) Uani 1 2 d DS T P
H1W H 0.570(3) 0.101(3) 0.729(2) 0.049 Uiso 1 1 d D U .
O2W O 0.32076(17) 0.61050(14) 0.50634(13) 0.0251(3) Uani 1 1 d D . .
H2W1 H 0.349(3) 0.619(3) 0.4506(16) 0.038 Uiso 1 1 d D U .
H2W2 H 0.308(3) 0.6798(18) 0.520(2) 0.038 Uiso 1 1 d D U .
O3W O 0.03607(18) 0.38527(15) 0.48145(13) 0.0325(4) Uani 1 1 d D . .
H3W1 H 0.056(4) 0.330(2) 0.444(2) 0.049 Uiso 1 1 d D U .
H3W2 H -0.035(3) 0.372(3) 0.514(2) 0.049 Uiso 1 1 d D U .
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'
Cu Cu 0.3201 1.2651 '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'
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
O1 C1 O2 122.3(2) . .
O1 C1 C2 119.07(18) . .
O2 C1 C2 118.60(19) . .
C1 C2 C3 112.84(17) . .
C1 C2 C4 110.80(18) . .
C3 C2 C4 109.44(18) . .
C1 C2 H2 107.9 . .
C3 C2 H2 107.9 . .
C4 C2 H2 107.9 . .
O3 C3 O4 121.6(2) . .
O3 C3 C2 118.13(19) . .
O4 C3 C2 120.20(18) . .
C5 C4 C2 113.9(2) . .
C5 C4 H4A 108.8 . .
C2 C4 H4A 108.8 . .
C5 C4 H4B 108.8 . .
C2 C4 H4B 108.8 . .
H4A C4 H4B 107.7 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
O4 Cu1 O4 174.01(10) . 3_656
O4 Cu1 O1W 87.00(5) . .
O4 Cu1 O1W 87.00(5) 3_656 .
O4 Cu1 O2 90.87(6) . .
O4 Cu1 O2 92.35(7) 3_656 .
O1W Cu1 O2 122.46(5) . .
O4 Cu1 O2 92.35(7) . 3_656
O4 Cu1 O2 90.87(7) 3_656 3_656
O1W Cu1 O2 122.47(5) . 3_656
O2 Cu1 O2 115.07(10) . 3_656
O3W Cu2 O3W 90.65(11) . 4_566
O3W Cu2 O2W 92.55(7) . 4_566
O3W Cu2 O2W 174.35(8) 4_566 4_566
O3W Cu2 O2W 174.35(8) . .
O3W Cu2 O2W 92.55(8) 4_566 .
O2W Cu2 O2W 84.65(11) 4_566 .
O3W Cu2 O1 83.96(7) . 4_566
O3W Cu2 O1 96.54(7) 4_566 4_566
O2W Cu2 O1 88.43(7) 4_566 4_566
O2W Cu2 O1 91.04(7) . 4_566
O3W Cu2 O1 96.54(7) . .
O3W Cu2 O1 83.97(7) 4_566 .
O2W Cu2 O1 91.04(7) 4_566 .
O2W Cu2 O1 88.43(7) . .
O1 Cu2 O1 179.28(8) 4_566 .
C1 O1 Cu2 125.01(14) . .
C1 O2 Cu1 127.18(14) . .
C3 O4 Cu1 126.11(14) . .
Cu1 O1W H1W 118(2) . .
Cu2 O2W H2W1 107(2) . .
Cu2 O2W H2W2 123(2) . .
H2W1 O2W H2W2 99(3) . .
Cu2 O3W H3W1 117(2) . .
Cu2 O3W H3W2 129(2) . .
H3W1 O3W H3W2 112(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.246(3) .
C1 O2 1.275(3) .
C1 C2 1.525(3) .
C2 C3 1.525(3) .
C2 C4 1.540(3) .
C2 H2 1.01(3) .
C3 O3 1.237(3) .
C3 O4 1.277(3) .
C4 C5 1.516(3) .
C4 H4A 0.97(2) .
C4 H4B 0.97(2) .
C5 H5A 0.94(2) .
C5 H5B 0.94(2) .
C5 H5C 0.94(2) .
Cu1 O4 1.9477(14) .
Cu1 O4 1.9477(14) 3_656
Cu1 O1W 1.999(2) .
Cu1 O2 2.0209(15) .
Cu1 O2 2.0210(15) 3_656
Cu2 O3W 1.9700(17) .
Cu2 O3W 1.9700(17) 4_566
Cu2 O2W 1.9727(17) 4_566
Cu2 O2W 1.9727(17) .
Cu2 O1 2.3936(14) 4_566
Cu2 O1 2.3936(14) .
O1W H1W 0.86(2) .
O2W H2W1 0.85(2) .
O2W H2W2 0.86(2) .
O3W H3W1 0.88(2) .
O3W H3W2 0.87(2) .
