#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:09:21 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178937 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/66/4116686.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_4116686
loop_
_publ_author_name
'Dianna M. Young'
'Urs Geiser'
'Arthur J. Schultz'
'H. Hau Wang'
_publ_contact_author
;
Dr. Arthur J. Schultz
Intense Pulsed Neutron Source
Argonne National Laboratory
9700 South Cass Avenue
Argonne, IL 60439, USA
;
_publ_contact_author_email       ajschultz@anl.gov
_publ_contact_author_fax         '(630) 252-4163'
_publ_contact_author_phone       '(630) 252-3465'
_publ_section_title
;
 Hydrothermal Synthesis of a Dense Metal-Organic Layered Framework That
 Contains Cu(I)-Olefinic Bonds, Cu2(O2CCHCHCO2)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1331
_journal_page_last               1332
_journal_paper_doi               10.1021/ja973483o
_journal_volume                  120
_journal_year                    1998
_chemical_compound_source        'Hydrothermal synthesis'
_chemical_formula_moiety         '(Cu+)2 (C4 H2 O4 2-)'
_chemical_formula_sum            'C12 H6 Cu6 O12'
_chemical_formula_weight         723.41
_chemical_name_common            'Copper(I) Fumarate'
_chemical_name_systematic
; 
 Copper(I) Fumarate'
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.298(2)
_cell_angle_beta                 96.627(2)
_cell_angle_gamma                104.739(2)
_cell_formula_units_Z            1
_cell_length_a                   5.1085(2)
_cell_length_b                   8.4464(4)
_cell_length_c                   9.0987(4)
_cell_measurement_reflns_used    1378
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.00
_cell_volume                     370.92(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method       'Area detector ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2182
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    8.522
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.239
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.619
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.011
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_obs          0.0554
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0812P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1428
_refine_ls_wR_factor_obs         0.1288
_reflns_number_observed          1175
_reflns_number_total             1592
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja973483o.cif
_cod_data_source_block           fumarate
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+0.0000P] 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^)+(0.0812P)^2^+0.0000P] 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               4116686
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.2625(2) 0.55171(11) 0.39759(11) 0.0198(3) Uani 1 d .
Cu2 Cu 0.5213(2) 0.08856(12) 0.15832(13) 0.0269(3) Uani 1 d .
Cu3A Cu -0.0630(4) -0.0445(2) 0.2688(2) 0.0171(7) Uani 0.505(5) d P
Cu3B Cu -0.1121(4) -0.0638(2) 0.1400(3) 0.0274(9) Uani 0.496(5) d P
C1 C 0.3923(15) 0.7492(9) 0.1728(8) 0.017(2) Uani 1 d .
C2 C 0.1845(15) 0.5902(9) 0.1827(8) 0.018(2) Uani 1 d .
H2 H 0.0053(15) 0.5911(9) 0.1913(8) 0.022 Uiso 1 calc R
C3 C 0.2562(15) 0.4441(9) 0.1790(8) 0.016(2) Uani 1 d .
H3 H 0.4400(15) 0.4454(9) 0.1877(8) 0.019 Uiso 1 calc R
C4 C 0.0410(16) 0.2835(9) 0.1612(8) 0.017(2) Uani 1 d .
O1 O 0.3041(11) 0.8784(6) 0.1866(6) 0.0222(12) Uani 1 d .
O2 O 0.6327(11) 0.7475(6) 0.1605(6) 0.0218(12) Uani 1 d .
O3 O -0.2026(10) 0.2839(6) 0.1539(6) 0.0229(13) Uani 1 d .
O4 O 0.1215(11) 0.1499(6) 0.1586(7) 0.0242(13) Uani 1 d .
C5 C 0.0631(16) 0.2391(8) 0.5022(8) 0.015(2) Uani 1 d .
C6 C 0.1029(15) 0.0703(9) 0.5000(9) 0.019(2) Uani 1 d .
H6 H 0.2793(15) 0.0595(9) 0.4986(9) 0.022 Uiso 1 calc R
O5 O -0.1821(11) 0.2487(6) 0.4941(6) 0.0213(12) Uani 1 d .
O6 O 0.2688(11) 0.3613(6) 0.5090(6) 0.0187(11) Uani 1 d .
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'
O O 0.0106 0.0060 '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
O5 Cu1 O6 117.9(2) 2_566 .
O5 Cu1 C2 98.9(3) 2_566 .
O6 Cu1 C2 139.3(2) . .
O5 Cu1 C3 138.0(3) 2_566 .
O6 Cu1 C3 102.2(2) . .
C2 Cu1 C3 39.1(3) . .
O5 Cu1 O6 95.0(2) 2_566 2_666
O6 Cu1 O6 83.5(2) . 2_666
C2 Cu1 O6 111.6(3) . 2_666
C3 Cu1 O6 102.0(2) . 2_666
O3 Cu2 O1 167.7(2) 1_655 1_545
O3 Cu2 O4 108.9(2) 1_655 .
O1 Cu2 O4 81.7(2) 1_545 .
O3 Cu2 Cu3B 86.8(2) 1_655 1_655
O1 Cu2 Cu3B 83.2(2) 1_545 1_655
O4 Cu2 Cu3B 163.9(2) . 1_655
O3 Cu2 Cu3A 87.7(2) 1_655 1_655
O1 Cu2 Cu3A 80.3(2) 1_545 1_655
O4 Cu2 Cu3A 154.1(2) . 1_655
Cu3B Cu2 Cu3A 24.24(6) 1_655 1_655
O3 Cu2 Cu2 99.0(2) 1_655 2_655
O1 Cu2 Cu2 84.1(2) 1_545 2_655
O4 Cu2 Cu2 103.4(2) . 2_655
Cu3B Cu2 Cu2 69.35(7) 1_655 2_655
Cu3A Cu2 Cu2 93.07(6) 1_655 2_655
Cu3B Cu3A O2 62.4(2) . 1_445
Cu3B Cu3A O4 61.4(2) . .
O2 Cu3A O4 123.2(2) 1_445 .
Cu3B Cu3A C6 161.3(3) . .
O2 Cu3A C6 135.8(3) 1_445 .
O4 Cu3A C6 100.0(3) . .
Cu3B Cu3A C6 160.6(3) . 2_556
O2 Cu3A C6 98.9(3) 1_445 2_556
O4 Cu3A C6 135.8(3) . 2_556
C6 Cu3A C6 36.9(4) . 2_556
Cu3B Cu3A O1 75.7(2) . 1_545
O2 Cu3A O1 97.9(2) 1_445 1_545
O4 Cu3A O1 75.8(2) . 1_545
C6 Cu3A O1 101.8(2) . 1_545
C6 Cu3A O1 114.1(3) 2_556 1_545
Cu3B Cu3A Cu2 64.97(13) . 1_455
O2 Cu3A Cu2 77.0(2) 1_445 1_455
O4 Cu3A Cu2 73.02(15) . 1_455
C6 Cu3A Cu2 110.6(2) . 1_455
C6 Cu3A Cu2 107.9(2) 2_556 1_455
O1 Cu3A Cu2 138.0(2) 1_545 1_455
Cu3A Cu3B O2 83.9(2) . 1_445
Cu3A Cu3B O4 85.9(2) . .
O2 Cu3B O4 166.8(3) 1_445 .
Cu3A Cu3B O1 75.4(2) . 1_545
O2 Cu3B O1 104.9(2) 1_445 1_545
O4 Cu3B O1 80.6(2) . 1_545
Cu3A Cu3B Cu2 90.80(15) . 1_455
O2 Cu3B Cu2 88.1(2) 1_445 1_455
O4 Cu3B Cu2 83.6(2) . 1_455
O1 Cu3B Cu2 159.7(2) 1_545 1_455
O2 C1 O1 125.7(7) . .
O2 C1 C2 119.4(6) . .
O1 C1 C2 114.7(6) . .
C3 C2 C1 120.9(7) . .
C3 C2 Cu1 71.2(4) . .
C1 C2 Cu1 106.2(5) . .
C2 C3 C4 120.2(7) . .
C2 C3 Cu1 69.7(4) . .
C4 C3 Cu1 102.5(5) . .
O3 C4 O4 123.4(7) . .
O3 C4 C3 119.3(6) . .
O4 C4 C3 117.3(7) . .
C1 O1 Cu2 121.6(5) . 1_565
C1 O1 Cu3A 137.8(5) . 1_565
Cu2 O1 Cu3A 100.1(2) 1_565 1_565
C1 O1 Cu3B 136.9(5) . 1_565
Cu2 O1 Cu3B 95.8(2) 1_565 1_565
Cu3A O1 Cu3B 28.86(9) 1_565 1_565
C1 O2 Cu3B 120.8(5) . 1_665
C1 O2 Cu3A 116.3(5) . 1_665
Cu3B O2 Cu3A 33.72(13) 1_665 1_665
C4 O3 Cu2 121.0(5) . 1_455
C4 O4 Cu3B 124.5(5) . .
C4 O4 Cu3A 121.9(5) . .
Cu3B O4 Cu3A 32.71(12) . .
C4 O4 Cu2 135.8(5) . .
Cu3B O4 Cu2 99.6(2) . .
Cu3A O4 Cu2 96.2(2) . .
O6 C5 O5 124.3(6) . .
O6 C5 C6 119.2(7) . .
O5 C5 C6 116.5(6) . .
C6 C6 C5 124.5(9) 2_556 .
C6 C6 Cu3A 72.1(6) 2_556 .
C5 C6 Cu3A 100.9(5) . .
C6 C6 Cu3A 71.0(6) 2_556 2_556
C5 C6 Cu3A 99.8(5) . 2_556
Cu3A C6 Cu3A 143.1(4) . 2_556
C5 O5 Cu1 120.2(5) . 2_566
C5 O6 Cu1 123.3(5) . .
C5 O6 Cu1 139.9(5) . 2_666
Cu1 O6 Cu1 96.5(2) . 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O5 1.987(5) 2_566
Cu1 O6 2.027(5) .
Cu1 C2 2.039(8) .
Cu1 C3 2.057(7) .
Cu1 O6 2.335(5) 2_666
Cu2 O3 1.887(5) 1_655
Cu2 O1 1.909(5) 1_545
Cu2 O4 2.231(5) .
Cu2 Cu3B 2.535(2) 1_655
Cu2 Cu3A 2.798(2) 1_655
Cu2 Cu2 3.005(2) 2_655
Cu3A Cu3B 1.149(3) .
Cu3A O2 2.058(6) 1_445
Cu3A O4 2.120(6) .
Cu3A C6 2.160(8) .
Cu3A C6 2.173(8) 2_556
Cu3A O1 2.303(5) 1_545
Cu3A Cu2 2.798(2) 1_455
Cu3B O2 1.833(6) 1_445
Cu3B O4 1.866(5) .
Cu3B O1 2.306(5) 1_545
Cu3B Cu2 2.535(2) 1_455
C1 O2 1.249(9) .
C1 O1 1.278(8) .
C1 C2 1.507(10) .
C2 C3 1.370(10) .
C3 C4 1.487(10) .
C4 O3 1.240(9) .
C4 O4 1.294(8) .
O1 Cu2 1.909(5) 1_565
O1 Cu3A 2.303(5) 1_565
O1 Cu3B 2.306(5) 1_565
O2 Cu3B 1.833(6) 1_665
O2 Cu3A 2.058(6) 1_665
O3 Cu2 1.887(5) 1_455
C5 O6 1.260(9) .
C5 O5 1.270(9) .
C5 C6 1.488(9) .
C6 C6 1.371(14) 2_556
C6 Cu3A 2.173(8) 2_556
O5 Cu1 1.987(5) 2_566
O6 Cu1 2.335(5) 2_666
