Spectral, structural and theoretical study of the effects of thiocyanato and dicyanamido ligands on the geometry of PbII complexes containing a triazinic ligand
Marandi, Farzin; Moeini, Keyvan; Mardani, Zahra; Krautscheid, Harald; Acta Crystallographica Section C Structural Chemistry 75 (2019) –; doi:10.1107/S2053229619008301

data_2021700
_publ_section_title
;
 Spectral, structural and theoretical study of the effects of thiocyanato
 and dicyanamido ligands on the geometry of PbII complexes containing a
 triazinic ligand
;
_journal_coeditor_code           YP3186
_journal_issue                   8
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229619008301
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Pb2 (C2 N3)2 (N O3)2 (C16 H10 N4 O2)4]'
_chemical_formula_moiety         'C68 H40 N24 O14 Pb2'
_chemical_formula_sum            'C68 H40 N24 O14 Pb2'
_chemical_formula_weight         1831.62
_chemical_name_systematic
Di-\m-dicyanamido-\k^2^<i>N</i>^1^:<i>N</i>^5^;\k^2^<i>N</i>^5^:<i>N</i>^1^-bis{[5,6-bis(furan-2-yl)-3-(pyridin-2-yl-\k<i>N</i>)-1,2,4-triazine-\k<i>N</i>^2^](nitrato-\k^2^<i>O</i>,<i>O</i>')lead(II)}
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                66.834(5)
_cell_angle_beta                 80.260(6)
_cell_angle_gamma                67.514(5)
_cell_formula_units_Z            1
_cell_length_a                   10.5123(8)
_cell_length_b                   12.2682(8)
_cell_length_c                   15.6379(10)
_cell_measurement_reflns_used    22877
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      1.9
_cell_volume                     1712.8(2)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2016)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2016)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2016)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996),
ORTEP-3 for Windows (Farrugia, 2012) and
DIAMOND (Bergerhof <i>et al.</i>,  1996)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.926
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.994
_exptl_absorpt_correction_T_max  0.4511
_exptl_absorpt_correction_T_min  0.3103
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-AREA; Stoe & Cie, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       'block, fragment'
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.767
_refine_ls_extinction_coef       0.00200(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                6299
_reflns_number_total             7484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3186sup1.cif
_cod_data_source_block           2
_cod_database_code               2021700
_shelx_estimated_absorpt_t_min   0.290
_shelx_estimated_absorpt_t_max   0.420
_shelx_hkl_checksum              32430
_shelx_res_checksum              26639
_cod_database_fobs_code 2021700