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_4320757
_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 H14 Cu N4 O2'
_chemical_formula_weight         333.83
_chemical_name_common            '[Cu(dmppy)(py)]2'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.866(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1734(10)
_cell_length_b                   12.4461(19)
_cell_length_c                   12.2131(14)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      5.1
_cell_volume                     1384.4(3)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_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      138(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1943
_diffrn_reflns_theta_full        56.42
_diffrn_reflns_theta_max         56.42
_diffrn_reflns_theta_min         5.09
_diffrn_standards_decay_%        <1.9
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.322
_exptl_absorpt_correction_T_max  0.8732
_exptl_absorpt_correction_T_min  0.4886
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0011(2)
_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   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         1818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+1.7383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                1703
_reflns_number_total             1818
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic010523n_1.cif
_cod_data_source_block           mn1076b
_cod_depositor_comments
;

2020-11-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C28 H28 Cu2 N8 O4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     667.66
_cod_database_code               4320757