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_1513183
_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            'C68 H76.75 Cd5 Cl4 N36 O29.5'
_chemical_formula_weight         2574.20
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.948(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   45.815(12)
_cell_length_b                   13.880(3)
_cell_length_c                   16.375(4)
_cell_measurement_reflns_used    9694
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.49
_cell_volume                     9961(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.945
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0672
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73129
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.8853
_exptl_absorpt_correction_T_min  0.7536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             5123
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.393
_refine_diff_density_min         -1.461
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1220
_refine_ls_number_reflns         22359
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+43.7726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                18586
_reflns_number_total             22359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-397-144-151-1.cif
_cod_data_source_block           skkar32a
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C68 H76.75 Cd5 Cl4 N36 O29.50'
_cod_database_code               1513183