Crystal structure of tris(<i>trans</i>-1,2-cyclohexanediamine-κ^2^<i>N</i>,<i>N</i>')chromium(III) tetrachloridozincate chloride trihydrate from synchrotron data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 72 (2016) 671–674; doi:10.1107/S2056989016005788

data_2241647
_publ_section_title
;
 Crystal structure of
 tris(<i>trans</i>-1,2-cyclohexanediamine-\k^2^<i>N</i>,<i>N</i>')chromium(III)
 tetrachloridozincate chloride trihydrate from synchrotron data
;
_journal_coeditor_code           WM5284
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              671
_journal_page_last               674
_journal_paper_doi               10.1107/S2056989016005788
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Cr (C6 H14 N2)3] [Zn Cl4] Cl , 3H2 O'
_chemical_formula_moiety         'C18 H42  Cr N6, 3(H2 O), Zn Cl4, Cl'
_chemical_formula_sum            'C18 H48 Cl5 Cr N6 O3 Zn'
_chemical_formula_weight         691.24
_chemical_name_systematic
'Tris(<i>trans</i>-1,2-cyclohexanediamine-\k^2^<i>N</i>,<i>N</i>')chromium(III) tetrachloridozincate chloride trihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.87(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.594(2)
_cell_length_b                   13.075(3)
_cell_length_c                   22.384(5)
_cell_measurement_reflns_used    39315
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.547
_cell_measurement_theta_min      0.361
_cell_volume                     3044.9(12)
_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</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.62998
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23113
_diffrn_reflns_theta_full        22.209
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.735
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm Scalepack</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         8090
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0353P)^2^+1.5820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                7647
_reflns_number_total             8090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5284sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        3045.0(11)
_cod_database_code               2241647
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.945
_shelx_hkl_checksum              38140
_shelx_res_checksum              58966
_cod_database_fobs_code 2241647