A rare pentanuclear cadmium(II) complex and two new mononuclear zinc(II) complexes of pyrazole derived ditopic ligands - Synthesis, crystal structures and spectral studies
Saugata Konar; Atanu Jana; Kinsuk Das; Sangita Ray; James A. Golen; Arnold L. Rheingold; Susanta Kumar Kar; Inorganica Chimica Acta 397 (2013) 144–151; doi:10.1016/j.ica.2012.12.003

data_1513184
_publ_section_title
;
 A rare pentanuclear cadmium(II) complex and two new mononuclear zinc(II)
 complexes of pyrazole derived ditopic ligands - Synthesis, crystal
 structures and spectral studies
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              144
_journal_page_last               151
_journal_paper_doi               10.1016/j.ica.2012.12.003
_journal_volume                  397
_journal_year                    2013
_chemical_formula_sum            'C22 H26 Cl2 N12 O11 Zn'
_chemical_formula_weight         770.82
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                95.2900(10)
_cell_angle_beta                 96.499(2)
_cell_angle_gamma                108.4850(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4714(14)
_cell_length_b                   12.0739(14)
_cell_length_c                   13.8484(17)
_cell_measurement_reflns_used    6683
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.94
_cell_measurement_theta_min      2.49
_cell_volume                     1790.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21726
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.8059
_exptl_absorpt_correction_T_min  0.7430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1624
_reflns_number_gt                4893
_reflns_number_total             6476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-397-144-151-2.cif
_cod_data_source_block           sksk20
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1513184