Crystal structure of <i>trans</i>-diammine(1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>)chromium(III) tetrachloridozincate chloride monohydrate from synchrotron data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 72 (2016) 456–459; doi:10.1107/S205698901600356X

data_2241595
_publ_section_title
;
 Crystal structure of
 <i>trans</i>-diammine(1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)chromium(III)
 tetrachloridozincate chloride monohydrate from synchrotron data
;
_journal_coeditor_code           WM5272
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              456
_journal_page_last               459
_journal_paper_doi               10.1107/S205698901600356X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Cr (C10 H24 N4) (N H3)2] [Zn Cl4] Cl, H2 O '
_chemical_formula_moiety         'C10 H30 Cr N6 Zn Cl4, Cl, H2 O '
_chemical_formula_sum            'C10 H32 Cl5 Cr N6 O Zn'
_chemical_formula_weight         547.
_chemical_name_systematic
'<i>trans</i>-Diammine(1,4,8,11-tetraazacyclotetradecane-\k<i>N</i>^4^)chromium(III) tetrachloridozincate chloride monohydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                66.03(3)
_cell_angle_beta                 76.03(3)
_cell_angle_gamma                78.74(3)
_cell_formula_units_Z            4
_cell_length_a                   9.3980(19)
_cell_length_b                   14.876(3)
_cell_length_c                   17.981(4)
_cell_measurement_reflns_used    76389
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      33.612
_cell_measurement_theta_min      0.355
_cell_volume                     2215.7(10)
_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</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0294
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23883
_diffrn_reflns_theta_full        21.839
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.099
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       block
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.757
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         12905
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.1347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                11123
_reflns_number_total             12905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5272sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2215.6(10)
_cod_database_code               2241595
_shelx_estimated_absorpt_t_min   0.850
_shelx_estimated_absorpt_t_max   0.938
_shelx_hkl_checksum              69924
_shelx_res_checksum              93553
_cod_database_fobs_code 2241595