Crystal structure of bis[<i>trans</i>-(1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>)bis(thiocyanato-κ<i>N</i>)chromium(III)] tetrachloridozincate from synchrotron data
Moon, Dohyun; Ryoo, Keon Sang; Choi, Jong-Ha; Acta Crystallographica Section E 71 (2015) 540–543; doi:10.1107/S205698901500746X

data_2240596
_publ_section_title
;
 Crystal structure of
 bis[<i>trans</i>-(1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)bis(thiocyanato-\k<i>N</i>)chromium(III)]
 tetrachloridozincate from synchrotron data
;
_journal_coeditor_code           SJ5452
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              540
_journal_page_last               543
_journal_paper_doi               10.1107/S205698901500746X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Cr (N C S)2 (C10 H24 N4)]2 [Zn Cl4]'
_chemical_formula_moiety         '2(C12 H24 Cr N6 S2 +), Zn Cl4 2-'
_chemical_formula_sum            'C24 H48 Cl4 Cr2 N12 S4 Zn'
_chemical_formula_weight         944.15
_chemical_name_systematic
;Bis[<i>trans</i>-(1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)bis(thiocyanato-\k<i>N</i>)chromium(III)]
tetrachloridozincate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9990(16)
_cell_length_b                   16.532(3)
_cell_length_c                   15.430(3)
_cell_measurement_reflns_used    92486
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.349
_cell_volume                     2000.5(7)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL ADSC Quantum-210 ADX</i> (Arvai & Nielsen, 1983)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      260(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.971
_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  0.0179
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20982
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.410
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm</i> Scalepack; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.581
_refine_ls_extinction_coef       0.013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2014/7</i> (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0404P)^2^+0.6258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                5500
_reflns_number_total             5738
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5452sup1.cf
_cod_data_source_block           I
_cod_database_code               2240596
_shelx_estimated_absorpt_t_min   0.801
_shelx_estimated_absorpt_t_max   0.883
_shelx_hkl_checksum              34180
_shelx_res_checksum              2625
_cod_database_fobs_code 2240596