Structural and anti-oxidant properties of guanidinium pyrazole-3,5-dicarboxylates
Packiaraj, S.; Pushpaveni, A.; Govindarajan, S.; Rawson, J. M.; CrystEngComm 18 (2016) 7978–; doi:10.1039/C6CE00290K

data_7226451
_publ_section_title
;
 Structural and anti-oxidant properties of guanidinium
 pyrazole-3,5-dicarboxylates
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              7978
_journal_paper_doi               10.1039/C6CE00290K
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'H2 O, C5 H3 N2 O4, C H6 N3'
_chemical_formula_sum            'C6 H11 N5 O5'
_chemical_formula_weight         233.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-15
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-08-25 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.503(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.7602(4)
_cell_length_b                   9.0277(4)
_cell_length_c                   17.1544(7)
_cell_measurement_reflns_used    4663
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      56.212
_cell_measurement_theta_min      4.771
_cell_volume                     1967.00(13)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker AXS Kappa Apex 2 CCD diffractomer'
_diffrn_measurement_method       'phi and omgea scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7327
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.314
_diffrn_reflns_theta_min         2.768
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.9732
_exptl_absorpt_correction_T_min  0.9601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2410
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.9335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2118
_reflns_number_total             2410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00290k2.cif
_cod_data_source_block           c1
_cod_depositor_comments
'Adding full bibliography for 7226450--7226453.cif.'
_cod_database_code               7226451
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.960
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups, All O(H) groups, All
  O(H,H) groups
2. Restrained distances
 O1S-H1SA = O1S-H1SB = O1-H1
 0.86 with sigma of 0.02
 N3-H3A = N3-H3B = N4-H4A = N4-H4B = N5-H5A = N5-H5B = N1-H1A
 0.86 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_shelx_res_checksum              82975
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'