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_7226452
_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         'C5 H2 N2 O4, 2(C H6 N3), H2 O, 1.58(O)'
_chemical_formula_sum            'C7 H19.16 N8 O6.59'
_chemical_formula_weight         320.83
_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             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                72.744(6)
_cell_angle_beta                 70.282(6)
_cell_angle_gamma                75.842(6)
_cell_formula_units_Z            2
_cell_length_a                   7.7868(14)
_cell_length_b                   10.0032(18)
_cell_length_c                   10.6058(19)
_cell_measurement_reflns_used    1893
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      55.309
_cell_measurement_theta_min      5.270
_cell_volume                     733.0(2)
_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    'SIR92 (Altomare et al. 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker AXS Kappa Apex II with CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3555
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         2.160
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.9672
_exptl_absorpt_correction_T_min  0.9619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2522
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0655P)^2^+0.0833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1949
_reflns_number_total             2522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00290k2.cif
_cod_data_source_block           rpg
_cod_depositor_comments
'Adding full bibliography for 7226450--7226453.cif.'
_cod_database_code               7226452
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N6-H6A
 0.86 with sigma of 0.02
 N6-H6B
 0.86 with sigma of 0.02
 N7-H7A
 0.86 with sigma of 0.02
 N7-H7B
 0.86 with sigma of 0.02
 H1SB-O1S = O1S-H1SA
 0.85 with sigma of 0.02
 H6A-H6B
 1.36 with sigma of 0.04
 H7A-H7B
 1.36 with sigma of 0.04
 H1SB-H1SA
 1.349 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O2AA) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: O1AA(0.75) O0AA(0.3333) O2AA(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2)
5.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N7(H7A,H7B), N8(H8A,H8B)
;
_shelx_res_checksum              90895
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'