Crystal structure of ammonium bis(pyridine-2,6-dicarboxylato-κ^3^<i>O</i>,<i>N</i>,<i>O</i>')chromate(III) from synchrotron data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 71 (2015) 210–212; doi:10.1107/S2056989015001152

data_2240411
_publ_section_title
;
 Crystal structure of ammonium
 bis(pyridine-2,6-dicarboxylato-\k^3^<i>O</i>,<i>N</i>,<i>O</i>')chromate(III)
 from synchrotron data
;
_journal_coeditor_code           SJ5438
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              210
_journal_page_last               212
_journal_paper_doi               10.1107/S2056989015001152
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(N H4) [Cr (C7 H3 N O4)2]'
_chemical_formula_moiety         'C14 H6 Cr N2 O8, N H4'
_chemical_formula_sum            'C14 H10 Cr N3 O8'
_chemical_formula_weight         400.25
_chemical_name_systematic
;
Bis(pyridine-2,6-dicarboxylato-\k^3^<i>O</i>,<i>N</i>,<i>O</i>')chromate(III)
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0305(10)
_cell_length_b                   7.0305(10)
_cell_length_c                   28.995(6)
_cell_measurement_reflns_used    20017
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      33.547
_cell_measurement_theta_min      0.361
_cell_volume                     1433.2(4)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL ADSC Quantum-210 ADX</i> (Arvai & Nielsen, 1983)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg, 2007)
;
_computing_publication_material
;
publCIF (Westrip 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2008, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.62998
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            6841
_diffrn_reflns_theta_full        22.209
_diffrn_reflns_theta_max         25.969
_diffrn_reflns_theta_min         4.038
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.861
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         943
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0461P)^2^+0.7347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                903
_reflns_number_total             943
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5438sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1433.2(5)
_cod_database_code               2240411
_cod_database_fobs_code          2240411
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.941
_shelx_hkl_checksum              49583
_shelx_res_checksum              61487