Crystal structure of tris[4-(dimethylamino)pyridinium] tris(oxalato-κ^2^<i>O</i>,<i>O</i>')chromate(III) tetrahydrate
Makon ma Houga, Noé; Capet, Frédéric; Nenwa, Justin; Bebga, Gouet; Foulon, Michel; Acta Crystallographica Section E 71 (2015) 1408–1410; doi:10.1107/S2056989015020113

data_2241265
_publ_section_title
;
 Crystal structure of tris[4-(dimethylamino)pyridinium]
 tris(oxalato-\k^2^<i>O</i>,<i>O</i>')chromate(III) tetrahydrate
;
_journal_coeditor_code           WM5230
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1408
_journal_page_last               1410
_journal_paper_doi               10.1107/S2056989015020113
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C7 H11 N2)3 [Cr (C3 O4)3], 4H2 O'
_chemical_formula_moiety         '3(C7 H11 N2 +), C6 Cr O12 3-, 4(H2 O)'
_chemical_formula_sum            'C27 H41 Cr N6 O16'
_chemical_formula_weight         757.66
_chemical_name_systematic
;
Tris[4-(dimethylamino)pyridinium]
tris(oxalato-\k^2^<i>O</i>,<i>O</i>')chromate(III) tetrahydrate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1141(5)
_cell_length_b                   16.7537(4)
_cell_length_c                   11.0053(2)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.35
_cell_volume                     3482.73(14)
_computing_cell_refinement
;
APEX2 (Bruker, 2014)
;
_computing_data_collection
;
SAINT (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009), publCIF (Westrip,
2010) and PLATON (Spek,
2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            56955
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.509
_diffrn_reflns_theta_min         2.601
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       prism
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.419
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5322
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0560P)^2^+1.5540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                3757
_reflns_number_total             5322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5230sup1.cif
_cod_data_source_block           I
_cod_database_code               2241265
_cod_database_fobs_code          2241265
_shelx_estimated_absorpt_t_min   0.798
_shelx_estimated_absorpt_t_max   0.945