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_1513185
_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 H30 Cl2 N14 O12 Zn'
_chemical_formula_weight         818.87
_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                101.5930(10)
_cell_angle_beta                 97.9330(10)
_cell_angle_gamma                94.9240(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7107(6)
_cell_length_b                   12.0150(6)
_cell_length_c                   12.1097(6)
_cell_measurement_reflns_used    7188
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.33
_cell_volume                     1641.79(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.998
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18704
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.8653
_exptl_absorpt_correction_T_min  0.8261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         7319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.0762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                5554
_reflns_number_total             7319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-397-144-151-3.cif
_cod_data_source_block           skkar39
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1513185