(1,4,8,11-Tetraazacyclotetradecane)palladium(II) diiodide monohydrate
Ha, Kwang; IUCrData 4 (2019) x191032–; doi:10.1107/S2414314619010320

data_1552130
_publ_section_title
;
 (1,4,8,11-Tetraazacyclotetradecane)palladium(II) diiodide monohydrate
;
_journal_coeditor_code           WM4111
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x191032
_journal_paper_doi               10.1107/S2414314619010320
_journal_volume                  4
_journal_year                    2019
_chemical_formula_iupac          '[Pd (C10 H24 N4)] I2 ,H2 O'
_chemical_formula_moiety         'C10 H24 N4 Pd, 2(I), H2 O'
_chemical_formula_sum            'C10 H26 I2 N4 O Pd'
_chemical_formula_weight         578.55
_chemical_name_systematic
;
(1,4,8,11-Tetraazacyclotetradecane)palladium(II) diiodide monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.9017(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3993(4)
_cell_length_b                   13.7266(5)
_cell_length_c                   13.8797(6)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.54
_cell_volume                     1786.61(13)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48072
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.086
_diffrn_reflns_theta_min         2.089
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.492
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2016)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.151
_exptl_crystal_description       Block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.716
_refine_ls_extinction_coef       0.00940(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0174
_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^)+(0.0147P)^2^+1.4653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0406
_reflns_number_gt                3307
_reflns_number_total             3544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4111sup1.cif
_cod_data_source_block           I
_cod_database_code               1552130
_cod_database_fobs_code          1552130
_shelx_estimated_absorpt_t_min   0.425
_shelx_estimated_absorpt_t_max   0.638
_shelx_hkl_checksum              14377
_shelx_res_checksum              52311