Crystal structure of 1,4,8,11-tetramethyl-1,4,8,11-tetraazoniacyclotetradecane bis[chloridochromate(VI)] dichloride from synchrotron X-ray data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 76 (2020) 523–526; doi:10.1107/S2056989020003059

data_2243313
_publ_section_title
;
 Crystal structure of
 1,4,8,11-tetramethyl-1,4,8,11-tetraazoniacyclotetradecane
 bis[chloridochromate(VI)] dichloride from synchrotron X-ray data
;
_journal_coeditor_code           VM2229
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              523
_journal_page_last               526
_journal_paper_doi               10.1107/S2056989020003059
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C14 H36 N4) [Cr O3 Cl]2 Cl2'
_chemical_formula_moiety         'C14 H36 N4 4+, 2(Cr O3 Cl -), 2(Cl -)'
_chemical_formula_sum            'C14 H36 Cl4 Cr2 N4 O6'
_chemical_formula_weight         602.27
_chemical_name_systematic
;
1,4,8,11-Tetramethyl-1,4,8,11-tetraazoniacyclotetradecane
bis[chloridochromate(VI)] dichloride
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                77.61(3)
_cell_angle_beta                 88.20(3)
_cell_angle_gamma                79.39(3)
_cell_formula_units_Z            1
_cell_length_a                   7.0610(14)
_cell_length_b                   8.6740(17)
_cell_length_c                   10.775(2)
_cell_measurement_reflns_used    41622
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.350
_cell_volume                     633.5(2)
_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>DIAMOND4</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6933
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.661
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm Scalepack</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.814
_refine_diff_density_min         -1.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1021P)^2^+0.4428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                3357
_reflns_number_total             3503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2229sup1.cif
_cod_data_source_block           I
_cod_database_code               2243313
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.911
_shelx_hkl_checksum              88671
_shelx_res_checksum              52901
_cod_database_fobs_code 2243313