Crystal structure of bis[<i>cis</i>-(1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>)(thiocyanato-κ<i>N</i>)chromium(III)] dichromate monohydrate from synchrotron X-ray diffraction data
Moon, Dohyun; Takase, Masahiro; Akitsu, Takashiro; Choi, Jong-Ha; Acta Crystallographica Section E 73 (2017) 72–75; doi:10.1107/S2056989016020120

data_2241991
_publ_section_title
;
 Crystal structure of
 bis[<i>cis</i>-(1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)(thiocyanato-\k<i>N</i>)chromium(III)]
 dichromate monohydrate from synchrotron X-ray diffraction data
;
_journal_coeditor_code           WM5351
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              72
_journal_page_last               75
_journal_paper_doi               10.1107/S2056989016020120
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Cr (N C S)2 (C10 H24 N4)]2 [Cr2 O7], H2 O'
_chemical_formula_moiety         'C24 H48 Cr2 N12 S4 2+, Cr2 O7 2-, H2 O'
_chemical_formula_sum            'C24 H50 Cr4 N12 O8 S4'
_chemical_formula_weight         971.00
_chemical_name_systematic
'Bis[<i>cis</i>-(1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)bis(thiocyanato-\k<i>N</i>)chromium(III)] dichromate monohydrate'
_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   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 93.335(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.044(2)
_cell_length_b                   16.221(2)
_cell_length_c                   15.041(2)
_cell_measurement_reflns_used    51334
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      33.612
_cell_measurement_theta_min      0.355
_cell_volume                     3907.8(9)
_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 4</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip,2010)
;
_computing_structure_refinement
;
<i>SHELXL2016</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      243(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     0.620
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11326
_diffrn_reflns_theta_full        21.839
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.559
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm Scalepack</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.733
_refine_ls_extinction_coef       0.0074(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2016/6 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5767
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0961P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                4156
_reflns_number_total             5767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5351sup1.cif
_cod_data_source_block           I
_cod_database_code               2241991
_cod_database_fobs_code          2241991
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.980
_shelx_hkl_checksum              27386
_shelx_res_checksum              44486