Aqua(1,4,7,10-tetraazacyclododecane)zinc(II) bis(perchlorate)
Ichimaru, Yoshimi; Kato, Koichi; Kurosaki, Hiromasa; Fujioka, Haruto; Sakai, Misa; Yamaguchi, Yoshihiro; Wanchun, Jin; Sugiura, Kirara; Imai, Masanori; Koike, Tohru; IUCrData 6 (2021) x210397–; doi:10.1107/S2414314621003977

data_1561946
_publ_section_title
;
 Aqua(1,4,7,10-tetraazacyclododecane)zinc(II) bis(perchlorate)
;
_journal_coeditor_code           VM4048
_journal_issue                   4
_journal_name_full               IUCrData
_journal_page_first              x210397
_journal_paper_doi               10.1107/S2414314621003977
_journal_volume                  6
_journal_year                    2021
_chemical_formula_iupac          '[Zn (C8 H20 N4) (H2 O)] (Cl O4)2'
_chemical_formula_moiety         'C8 H22 N4 O Zn 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C8 H22 Cl2 N4 O9 Zn'
_chemical_formula_weight         454.56
_chemical_name_systematic
;
Aqua(1,4,7,10-tetraazacyclododecane)zinc(II) bis(perchlorate)
;
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.881(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3428(6)
_cell_length_b                   8.4603(4)
_cell_length_c                   16.0543(6)
_cell_measurement_reflns_used    3951
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      68.1350
_cell_measurement_theta_min      5.4800
_cell_volume                     1674.33(13)
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro (Rigaku OD, 2020)'
_computing_molecular_graphics    '<i>OLEX2</i> (Dolomanov et al., 2009)'
_computing_publication_material  '<i>OLEX2</i> (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015<i>b</i>)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015<i>a</i>)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  Rigaku_Synergy-i
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7740
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.368
_diffrn_reflns_theta_min         3.586
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.478
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.844
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0991P)^2^+7.9372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.1856
_reflns_number_gt                2670
_reflns_number_total             3025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm4048sup1.cif
_cod_data_source_block           I
_cod_database_code               1561946
_cod_database_fobs_code          1561946
_shelx_hkl_checksum              41539
_shelx_res_checksum              56542