Crystal structure of <i>trans</i>-dichlorido(1,4,8,11-tetraazaundecane-κ^4^<i>N</i>)chromium(III) perchlorate determined from synchrotron data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 72 (2016) 424–427; doi:10.1107/S2056989016002978

data_2241584
_publ_section_title
;
 Crystal structure of
 <i>trans</i>-dichlorido(1,4,8,11-tetraazaundecane-\k^4^<i>N</i>)chromium(III)
 perchlorate determined from synchrotron data
;
_journal_coeditor_code           WM5269
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              424
_journal_page_last               427
_journal_paper_doi               10.1107/S2056989016002978
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Cr Cl2 (C7 H20 N4)] Cl O4'
_chemical_formula_moiety         'C7 H20 Cl2 Cr N4 +, Cl O4 -'
_chemical_formula_sum            'C7 H20 Cl3 Cr N4 O4'
_chemical_formula_weight         382.62
_chemical_name_systematic
;
<i>trans</i>-Dichlorido(1,4,8,11-tetraazaundecane-\k^4^<i>N</i>)chromium(III)
perchlorate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.42(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4730(13)
_cell_length_b                   11.449(2)
_cell_length_c                   10.385(2)
_cell_measurement_reflns_used    22325
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      33.612
_cell_measurement_theta_min      0.355
_cell_volume                     751.6(3)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC Program</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>SHELXL2014/7</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.620
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7831
_diffrn_reflns_theta_full        21.839
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.340
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       block
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.623
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2004 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.038(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4422
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0435P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                4214
_reflns_number_total             4422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5269sup1.cif
_cod_data_source_block           I
_cod_database_code               2241584
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.958
_shelx_hkl_checksum              7231
_shelx_res_checksum              27834
_cod_database_fobs_code 2241584