Crystal structure of bis-[(oxalato-κ<sup>2</sup><i>O</i><sup>1</sup>,<i>O</i><sup>2</sup>)(1,4,8,11-tetra-aza-cyclo-tetra-decane-κ<sup>4</sup><i>N</i>)chromium(III)] dichromate octa-hydrate from synchrotron X-ray data.
Moon, Dohyun; Choi, Jong-Ha; Acta crystallographica. Section E, Crystallographic communications 73 (2017) 403–406; doi:10.1107/S2056989017002614

data_2311358
_publ_section_title
;
 Crystal structure of
 bis-[(oxalato-\k<sup>2</sup><i>O</i><sup>1</sup>,<i>O</i><sup>2</sup>)(1,4,8,11-tetra-aza-cyclo-tetra-decane-\k<sup>4</sup><i>N</i>)chromium(III)]
 dichromate octa-hydrate from synchrotron X-ray data.
;
_journal_coeditor_code           SJ5521
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              403
_journal_page_last               406
_journal_paper_doi               10.1107/S2056989017002614
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Cr (C2 O4) (C10 H24 N4)]2 [Cr2 O7], 8H2 O'
_chemical_formula_moiety         '2(C12 H24 Cr N4 O4 +), Cr2 O7 2-, 8(H2 O)'
_chemical_formula_sum            'C24 H64 Cr4 N8 O23'
_chemical_formula_weight         1040.83
_chemical_name_systematic
'Bis[(oxalato-\k^2^<i>O</i>^1^,<i>O</i>^2^)(1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)chromium(III)] dichromate octahydrate'
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 100.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8270(16)
_cell_length_b                   15.407(3)
_cell_length_c                   18.086(4)
_cell_measurement_reflns_used    63673
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.349
_cell_volume                     2141.9(8)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC</i> (Shin <i>et al.</i>,  2016)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
<i>DIAMOND 4</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21270
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.272
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.618
_refine_diff_density_min         -0.692
_refine_ls_extinction_coef       0.037(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5775
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+1.1358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                4844
_reflns_number_total             5775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5521sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2311358
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.949
_shelx_hkl_checksum              35636
_shelx_res_checksum              91519