Crystal structure of 1,4,8,11-tetraazoniacyclotetradecane bis(dichromate) monohydrate from synchrotron data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 73 (2017) 755–758; doi:10.1107/S2056989017005771

data_2242149
_publ_section_title
;
 Crystal structure of 1,4,8,11-tetraazoniacyclotetradecane bis(dichromate)
 monohydrate from synchrotron data
;
_journal_coeditor_code           WM5385
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              755
_journal_page_last               758
_journal_paper_doi               10.1107/S2056989017005771
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '(C10 H28 N4) [Cr2 O7]2, H2 O'
_chemical_formula_moiety         'C10 H28 N4 4+, 2(Cr2 O7 2-), H2 O'
_chemical_formula_sum            'C10 H30 Cr4 N4 O15'
_chemical_formula_weight         654.38
_chemical_name_systematic
;
1,4,8,11-Tetraazoniacyclotetradecane bis(dichromate)
monohydrate
;
_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   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 94.671(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.428(2)
_cell_length_b                   13.961(2)
_cell_length_c                   15.490(2)
_cell_measurement_reflns_used    70448
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.349
_cell_volume                     2247.6(6)
_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</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2015</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2015</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0163
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12953
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         1.682
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm Scalepack</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.093
_refine_diff_density_max         2.213
_refine_diff_density_min         -1.044
_refine_ls_extinction_coef       0.0096(10)
_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   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6614
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0712P)^2^+4.2149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                5804
_reflns_number_total             6614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5385sup1.cif
_cod_data_source_block           I
_cod_database_code               2242149
_cod_database_fobs_code          2242149
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.890
_shelx_hkl_checksum              66029
_shelx_res_checksum              21514