Cadmium(II) complexes containing N,N´-dimethylvioluric acid as ligand or counteranion: Synthesis, characterization, crystal structures and DFT study
Frontera, Antonio; Banik, Rupak; Roy, Subhadip; Bauza, Antonio; Das, Subrata; RSC Adv.  (2015) –; doi:10.1039/C4RA10251G

data_7219221
_publ_section_title
;
 Cadmium(II) complexes containing N,N&#x00B4;-dimethylvioluric acid as
 ligand or counteranion: Synthesis, characterization, crystal structures
 and DFT study
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA10251G
_journal_year                    2015
_chemical_formula_moiety         '2(C6 H6 N3 O4), C10 H18 Cd N2 O4'
_chemical_formula_sum            'C22 H30 Cd N8 O12'
_chemical_formula_weight         710.94
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-04-17
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2014.04.04 svn.r2922, GUI svn.r3563)
;
_audit_update_record
;
2014-07-31 deposited with the CCDC.
2015-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                88.351(2)
_cell_angle_beta                 85.190(2)
_cell_angle_gamma                62.638(2)
_cell_formula_units_Z            1
_cell_length_a                   8.4597(5)
_cell_length_b                   9.1787(5)
_cell_length_c                   10.2999(6)
_cell_measurement_reflns_used    3341
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.998
_cell_measurement_theta_min      2.499
_cell_volume                     707.75(7)
_computing_data_collection       'Bruker Smart Apex II'
_computing_data_reduction        'Bruker SAINT (2001)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w scans and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12467
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.499
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  25.998
_exptl_absorpt_correction_T_min  2.499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       needle
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.8478
_exptl_transmission_factor_min   0.7008
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2766
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.0695P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2746
_reflns_number_total             2766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra10251g2.cif
_cod_data_source_block           3
_cod_database_code               7219221
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2WB-O2W = O2W-H2WA
 0.85 with sigma of 0.02
 H1WA-O1W = O1W-H1WB
 0.85 with sigma of 0.02
 H2WB-H2WA
 1.301 with sigma of 0.04
 H1WA-H1WB
 1.301 with sigma of 0.04
 O2W-H2WB \\sim O2W-H2WA \\sim O1W-H1WA \\sim O1W-H1WB
 with sigma of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7)
3.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              21261
_shelx_hkl_checksum              83508