Synthesis, crystal structure and properties of trigonal bipyramidal [M(L5)2(H2O)]·H2O complexes [M = cobalt(II) (S = 3/2) or copper(II) (S = 1/2); HL5 = N-(2-chloro-6-methylphenyl)pyridine-2-carboxamide]
Patra, Apurba Kumar; Ray, Manabendra; Mukherjee, Rabindranath; Journal of the Chemical Society, Dalton Transactions  (1999) 2461–; doi:10.1039/a902851j

data_7027445
_publ_contact_author
;
     ? name             Prof. R. Mukherjee
     ? institute        Indian Institute of Technology Kanpur
     ? department       Department of Chemistry
     ? address          208 016
     ? city             Kanpur
     ? country          India
;
_publ_section_title
;
 Synthesis, crystal structure and properties of trigonal bipyramidal
 [M(L5)2(H2O)]&#x00B7;H2O complexes [M&#x2005;=&#x2005;cobalt(II)
 (S&#x2005;=&#x2005;3/2) or copper(II) (S&#x2005;=&#x2005;1/2);
 HL5&#x2005;=&#x2005;N-(2-chloro-6-methylphenyl)pyridine-2-carboxamide]
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2461
_journal_paper_doi               10.1039/a902851j
_journal_year                    1999
_chemical_compound_source        'Synthesized in the laboratory'
_chemical_formula_analytical     'C26 H24 N4 O4 Cl2 Cu'
_chemical_formula_moiety         '((C26 H22 N4 O3 Cl2(2-) Cu(2+))(2H O)'
_chemical_formula_structural
'[(C13 H10 N2 O Cl)(C13 H10 N2 O Cl) Cu(2H O)](2H O)'
_chemical_formula_sum            'C26 H24 Cl2 Cu N4 O4'
_chemical_formula_weight         590.5
_chemical_melting_point          'Decomposed above 280 degree celcius'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   'Positions calculated'
_atom_sites_solution_primary     'Cu,N atoms'
_atom_sites_solution_secondary   'Rest non hydrogen atoms'
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            8
_cell_length_a                   21.139(7)
_cell_length_b                   15.858(6)
_cell_length_c                   15.665(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      23.86
_cell_measurement_theta_min      8.98
_cell_volume                     5251(3)
_computing_data_collection       'CAD4mach- PC Version     '
_computing_data_reduction        xtal_DIFDAT_SORTRF_ADDREF_ABSORB
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal_SIMPEL
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'CAD4 Mach   '
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_detector       'proportional counter     '
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_source         'Sealed xray_tube  '
_diffrn_radiation_type           'Mo K-alpha      '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .032
_diffrn_reflns_av_sigmaI/netI    .038
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9967
_diffrn_reflns_reduction_process No_monochr_Lp_applied
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0.46%
_diffrn_standards_interval_time  'every hour '
_diffrn_standards_number         three
_exptl_absorpt_coefficient_mu    1.08/mm
_exptl_absorpt_correction_T_max  0.7417
_exptl_absorpt_correction_T_min  0.7400
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_meas      1.510
_exptl_crystal_density_method    Flotation
_exptl_crystal_description       'Rectangular parallelopiped   '
_exptl_crystal_F_000             2423.53
_exptl_crystal_preparation
'Slow evaporation of methanol/water(1:1) solution of the complex'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         .824
_refine_diff_density_min         -.685
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.569
_refine_ls_goodness_of_fit_obs   3.023
_refine_ls_hydrogen_treatment    no
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2771
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .097
_refine_ls_R_factor_obs          .056
_refine_ls_shift/esd_max         0.2873x10-3
_refine_ls_shift/esd_mean        0.3081x10-4
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .06
_refine_ls_wR_factor_obs         .054
_reflns_d_resolution_high        .833
_reflns_d_resolution_low         10.57
_reflns_limit_h_max              25
_reflns_limit_h_min              0
_reflns_limit_k_max              0
_reflns_limit_k_min              -18
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_observed          2779
_reflns_number_total             4618
_reflns_observed_criterion       ' refl_observed_if_Inet_>_.000_sigma(Inet)'
_cod_data_source_file            902851jsup1.cif
_cod_data_source_block           cu
_cod_original_cell_volume        5251.26(3)
_cod_original_sg_symbol_Hall     -P_2ac_2ab
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C26 H24 N4 O4 Cl2 Cu'
_cod_database_code               7027445