Structure-Spectroscopy Correlation in Distorted Five-Coordinate Cu(II) Complexes: A Case Study with a Set of Closely Related Copper Complexes of Pyridine-2,6-dicarboxamide Ligands
Dana S. Marlin; Marilyn M. Olmstead; Pradip K. Mascharak; Inorganic Chemistry 40 (2001) 7003–7008; doi:10.1021/ic010523n

data_4320759
_publ_section_title
;
 Structure-Spectroscopy Correlation in Distorted Five-Coordinate Cu(II)
 Complexes: A Case Study with a Set of Closely Related Copper Complexes of
 Pyridine-2,6-dicarboxamide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7003
_journal_page_last               7008
_journal_paper_doi               10.1021/ic010523n
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C14 H16 Cu N4 O3'
_chemical_formula_weight         351.85
_chemical_name_common            '[Cu(dmppy)(H2O)(py)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.5090(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6463(6)
_cell_length_b                   10.5912(8)
_cell_length_c                   16.5888(12)
_cell_measurement_reflns_used    6319
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      2.3
_cell_volume                     1512.10(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20322
_diffrn_reflns_theta_full        31.43
_diffrn_reflns_theta_max         31.43
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    1.462
_exptl_absorpt_correction_T_max  0.8920
_exptl_absorpt_correction_T_min  0.5924
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, Sheldrick, G.M. An empirical absorption correction program based
  on the method of Blessing, R. H., Acta Cryst. (1995). A51, 33-38.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.068
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.1647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                4243
_reflns_number_total             4734
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic010523n_3.cif
_cod_data_source_block           mn1039
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4320759