Flexible Square Supramolecular Rings with Hydrogen-Bonded Bushing in Solid-State Oxalurate Complexes: Versatility of the Oxalurate Ligand in Covalent and Noncovalent Binding
Larry R. Falvello; Raquel Garde; Milagros Tomás; Inorganic Chemistry 41 (2002) 4599–4604; doi:10.1021/ic025648m

data_4318422
_publ_section_title
;
 Flexible Square Supramolecular Rings with Hydrogen-Bonded Bushing in
 Solid-State Oxalurate Complexes: Versatility of the Oxalurate Ligand in
 Covalent and Noncovalent Binding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4599
_journal_page_last               4604
_journal_paper_doi               10.1021/ic025648m
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C6 H14 Cu N4 O12'
_chemical_formula_weight         397.75
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.69(2)
_cell_angle_beta                 83.39(2)
_cell_angle_gamma                71.266(16)
_cell_formula_units_Z            1
_cell_length_a                   5.2584(8)
_cell_length_b                   6.8332(15)
_cell_length_c                   10.314(2)
_cell_measurement_temperature    148(2)
_cell_volume                     334.99(12)
_computing_cell_refinement       'CAD4/PC V2.0 (Nonius, 1996)'
_computing_data_collection       'CAD4/PC V2.0 (Nonius, 1996)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_molecular_graphics    'SHELXTL Rel. 5.05/V (Siemens, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      148(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       omega-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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1704
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  0.8897
_exptl_absorpt_correction_T_min  0.6845
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             203
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    independent
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.2150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                1432
_reflns_number_total             1534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025648m_s1_3.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
 Correcting the way multiline values are recorded in the _audit_author loop.

 Antanas Vaitkus,
 2018-07-07

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.2150P] 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^)+(0.0414P)^2^+0.2150P] 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        334.99(11)
_cod_database_code               4318422