Crystal structure of <i>trans</i>-bis(ethane-1,2-diamine-κ^2^<i>N</i>,<i>N</i>')bis(thiocyanato-κ<i>N</i>)chromium(III) perchlorate from synchrotron data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 71 (2015) 650–653; doi:10.1107/S2056989015009184

data_2240743
_publ_section_title
;
 Crystal structure of
 <i>trans</i>-bis(ethane-1,2-diamine-\k^2^<i>N</i>,<i>N</i>')bis(thiocyanato-\k<i>N</i>)chromium(III)
 perchlorate from synchrotron data
;
_journal_coeditor_code           SJ5459
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              650
_journal_page_last               653
_journal_paper_doi               10.1107/S2056989015009184
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Cr (N C S)2 (C2 H8 N2)2] Cl O4'
_chemical_formula_moiety         'C6 H16  Cr N6 S2 +, Cl O4 -'
_chemical_formula_sum            'C6 H16 Cl Cr N6 O4 S2'
_chemical_formula_weight         387.82
_chemical_name_systematic
'<i>trans</i>-Bis(ethane-1,2-diamine-\k^2^<i>N</i>,<i>N</i>')bis(thiocyanato-\k<i>N</i>)chromium(III) perchlorate'
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.83(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.599(3)
_cell_length_b                   7.4440(15)
_cell_length_c                   13.792(3)
_cell_measurement_reflns_used    46962
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_volume                     1540.8(6)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL ADSC Quantum-210 ADX Program </i>(Arvai & Nielsen, 1983)
;
_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>SHELXT2014/5</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      260(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8172
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.707
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEAPCK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.735
_refine_diff_density_min         -1.119
_refine_ls_extinction_coef       0.045(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014/7 (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0599
_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^)+(0.1146P)^2^+2.4721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1763
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                2019
_reflns_number_total             2121
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5459sup1.cf
_cod_data_source_block           I
_cod_database_code               2240743
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.897
_shelx_hkl_checksum              34793
_shelx_res_checksum              75565
_cod_database_fobs_code 2240743