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_7219219
_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         'C6 H7 N3 O4, H2 O'
_chemical_formula_sum            'C6 H9 N3 O5'
_chemical_formula_weight         203.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-03-05
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2014-07-31 deposited with the CCDC.
2015-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.314(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3766(8)
_cell_length_b                   6.2427(6)
_cell_length_c                   17.4768(17)
_cell_measurement_reflns_used    3231
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.995
_cell_measurement_theta_min      2.386
_cell_volume                     892.88(15)
_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)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0238
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         2.386
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.6982
_exptl_absorpt_correction_T_min  0.6492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       needle
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         1753
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+0.2716P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1480
_reflns_number_total             1753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra10251g2.cif
_cod_data_source_block           1
_cod_database_code               7219219
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 N1B-C1 \\sim N1B-C1
 with sigma of 0.001
 N1B-O1B \\sim N1A-O1A
 with sigma of 0.001
 N1B-C1 \\sim N1A-C1
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(N1A) = Uanis(N1B)
4. Others
 Uiso(H3A)=Uiso(H3B)=Uiso(H3C)=FVAR(1)
 Uiso(H5A)=Uiso(H5B)=Uiso(H5C)=FVAR(2)
 Sof(O1B)=Sof(H1B)=Sof(N1B)=1-FVAR(3)
 Sof(O1A)=Sof(H1A)=Sof(N1A)=FVAR(3)
5.a Riding coordinates:
 O1A(H1A), O1B(H1B), O5(H5D,H5E)
5.b Rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              35875
_shelx_hkl_checksum              11118
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'