First crystal structures of metal complexes with a 4-nitropyrazole-3-carboxylic acid ligand and the third crystal form of the ligand
Jaćimović, Željko K.; Novaković, Sladjana B.; Bogdanović, Goran A.; Giester, Gerald; Kosović, Milica; Libowitzky, Eugen; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619001244

data_2021476
_publ_section_title
;
 First crystal structures of metal complexes with a
 4-nitropyrazole-3-carboxylic acid ligand and the third crystal form of
 the ligand
;
_journal_coeditor_code           YO3057
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619001244
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Co2 (C4 H1 N3 O4)2 (H2 O1)6], 2H2 O'
_chemical_formula_moiety         'C8 H14 Co2 N6 O14, 2(H2 O)'
_chemical_formula_sum            'C8 H18 Co2 N6 O16'
_chemical_formula_weight         572.14
_chemical_name_systematic
'Bis(\m-4-nitro-1<i>H</i>-imidazol-1-ide-5-carboxylato)-\k^2^<i>N</i>^1^,<i>O</i>:<i>N</i>^2^;\k^2^<i>N</i>^2^:<i>N</i>^1^,<i>O</i>-bis[triaquacobalt(II)] dihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 102.930(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9689(11)
_cell_length_b                   6.4035(8)
_cell_length_c                   16.4509(19)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      66.542
_cell_measurement_theta_min      4.782
_cell_volume                     920.86(19)
_computing_cell_refinement
;
APEX2 (Bruker, 2008)
;
_computing_data_collection
;
SAINT (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker ApexII CCD'
_diffrn_measurement_method       'phi and omegas scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32322
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.289
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'Incoatec ImS'
_exptl_absorpt_coefficient_mu    1.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_description       prism
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.231
_refine_ls_extinction_coef       0.0055(6)
_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   1.065
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0219P)^2^+0.4119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0486
_reflns_number_gt                3366
_reflns_number_total             3531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yo3057sup1.cif
_cod_data_source_block           III
_cod_database_code               2021476
_cod_database_fobs_code          2021476
_shelx_hkl_checksum              96424
_shelx_res_checksum              28890
_shelxl_version_number           2014/6