Hydrothermal Synthesis of a Dense Metal-Organic Layered Framework That Contains Cu(I)-Olefinic Bonds, Cu2(O2CCHCHCO2)
Dianna M. Young; Urs Geiser; Arthur J. Schultz; H. Hau Wang; Journal of the American Chemical Society 120 (1998) 1331–1332; doi:10.1021/ja973483o

data_4116686
_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 \w 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/[\s^2^(Fo^2^)+(0.0812P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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