Crystal structure of <i>cis</i>-aquachlorido(<i>rac</i>-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ^4^<i>N</i>)chromium(III) tetrachloridozincate trihydrate from synchrotron data
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 71 (2015) 1054–1057; doi:10.1107/S2056989015015212

data_2241036
_publ_section_title
;
 Crystal structure of
 <i>cis</i>-aquachlorido(<i>rac</i>-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)chromium(III)
 tetrachloridozincate trihydrate from synchrotron data
;
_journal_coeditor_code           WM5196
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1054
_journal_page_last               1057
_journal_paper_doi               10.1107/S2056989015015212
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Cr Cl (C16 H38 N4 O) (H2 O)] [Zn Cl4] 3H2 O'
_chemical_formula_moiety         'C16 H38 Cl Cr N4 O, Zn Cl4, 3(H2 O)'
_chemical_formula_sum            'C16 H44 Cl5 Cr N4 O4 Zn'
_chemical_formula_weight         651.17
_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   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                81.73(3)
_cell_angle_beta                 75.80(3)
_cell_angle_gamma                74.90(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1010(18)
_cell_length_b                   9.5830(19)
_cell_length_c                   17.007(3)
_cell_measurement_reflns_used    68409
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.349
_cell_volume                     1383.2(5)
_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
;
<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 0.962
_diffrn_measured_fraction_theta_max 0.960
_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  0.0127
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14317
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.252
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEAPCK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       plate
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.555
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         7413
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0439P)^2^+0.7948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                7053
_reflns_number_total             7413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5196sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1383.2(6)
_cod_database_code               2241036
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.917
_shelx_hkl_checksum              33087
_shelx_res_checksum              94121
_cod_database_fobs_code 2241036