#------------------------------------------------------------------------------
#$Date: 2020-11-05 10:56:28 +0200 (Thu, 05 Nov 2020) $
#$Revision: 258736 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/07/4320757.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320757
loop_
_publ_author_name
'Dana S. Marlin'
'Marilyn M. Olmstead'
'Pradip K. Mascharak'
_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'
_chemical_name_systematic
;
  ?
;
_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       2θ-ω
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0573P)²+1.7383P] where P=(Fo²+2Fc²)/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     >2σ(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_formula_sum            'C28 H28 Cu2 N8 O4'
_cod_original_formula_weight         667.66
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4320757
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.24102(5) 0.99107(3) 0.07208(3) 0.0168(2) Uani 1 1 d . . .
O1 O -0.0220(2) 0.74501(17) -0.04957(18) 0.0247(5) Uani 1 1 d . . .
O2 O 0.5074(2) 1.13528(15) -0.12698(16) 0.0198(5) Uani 1 1 d . . .
N1 N 0.0903(3) 0.8757(2) 0.06729(19) 0.0195(6) Uani 1 1 d . . .
N2 N 0.2450(3) 0.9422(2) -0.07688(18) 0.0168(6) Uani 1 1 d . . .
N3 N 0.3665(3) 1.10617(19) 0.01612(19) 0.0161(6) Uani 1 1 d . . .
N4 N 0.2508(3) 1.02859(19) 0.23050(19) 0.0162(6) Uani 1 1 d . . .
C1 C 0.0011(3) 0.8418(3) 0.1526(3) 0.0261(7) Uani 1 1 d . . .
H1A H -0.1027 0.8411 0.1222 0.039 Uiso 1 1 calc R . .
H1B H 0.0153 0.8921 0.2148 0.039 Uiso 1 1 calc R . .
H1C H 0.0308 0.7696 0.1782 0.039 Uiso 1 1 calc R . .
C2 C 0.0667(3) 0.8202(2) -0.0264(2) 0.0193(7) Uani 1 1 d . . .
C3 C 0.1613(3) 0.8587(2) -0.1120(2) 0.0179(7) Uani 1 1 d . . .
C4 C 0.1630(3) 0.8198(2) -0.2173(2) 0.0198(7) Uani 1 1 d . . .
H4 H 0.1045 0.7599 -0.2430 0.024 Uiso 1 1 calc R . .
C5 C 0.2536(3) 0.8713(2) -0.2853(2) 0.0220(7) Uani 1 1 d . . .
H5 H 0.2571 0.8462 -0.3584 0.026 Uiso 1 1 calc R . .
C6 C 0.3387(3) 0.9593(3) -0.2466(2) 0.0195(7) Uani 1 1 d . . .
H6 H 0.3993 0.9953 -0.2927 0.023 Uiso 1 1 calc R . .
C7 C 0.3328(3) 0.9924(2) -0.1401(3) 0.0161(7) Uani 1 1 d . . .
C8 C 0.4119(3) 1.0863(2) -0.0807(2) 0.0157(7) Uani 1 1 d . . .
C9 C 0.4230(3) 1.2040(2) 0.0719(2) 0.0207(7) Uani 1 1 d . . .
H9A H 0.5189 1.2216 0.0489 0.031 Uiso 1 1 calc R . .
H9B H 0.4334 1.1928 0.1519 0.031 Uiso 1 1 calc R . .
H9C H 0.3545 1.2633 0.0524 0.031 Uiso 1 1 calc R . .
C10 C 0.1977(3) 1.1218(2) 0.2656(2) 0.0178(7) Uani 1 1 d . . .
H10 H 0.1588 1.1730 0.2122 0.021 Uiso 1 1 calc R . .
C11 C 0.1975(3) 1.1459(2) 0.3751(2) 0.0208(7) Uani 1 1 d . . .
H11 H 0.1568 1.2115 0.3968 0.025 Uiso 1 1 calc R . .
C12 C 0.2575(3) 1.0733(3) 0.4533(3) 0.0235(7) Uani 1 1 d . . .
H12 H 0.2604 1.0890 0.5296 0.028 Uiso 1 1 calc R . .
C13 C 0.3134(3) 0.9771(2) 0.4188(2) 0.0202(7) Uani 1 1 d . . .
H13 H 0.3554 0.9259 0.4710 0.024 Uiso 1 1 calc R . .
C14 C 0.3070(3) 0.9574(2) 0.3074(2) 0.0189(7) Uani 1 1 d . . .
H14 H 0.3437 0.8910 0.2838 0.023 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 N4 173.98(10) . . ?
N2 Cu1 N1 80.56(10) . . ?
N4 Cu1 N1 98.56(10) . . ?
N2 Cu1 N3 80.03(10) . . ?
N4 Cu1 N3 101.73(9) . . ?
N1 Cu1 N3 158.37(10) . . ?
C2 N1 C1 114.5(2) . . ?
C2 N1 Cu1 116.16(19) . . ?
C1 N1 Cu1 129.3(2) . . ?
C3 N2 C7 122.9(2) . . ?
C3 N2 Cu1 118.42(19) . . ?
C7 N2 Cu1 118.7(2) . . ?
C8 N3 C9 116.2(2) . . ?
C8 N3 Cu1 115.17(19) . . ?
C9 N3 Cu1 128.47(18) . . ?
C14 N4 C10 117.8(2) . . ?
C14 N4 Cu1 119.6(2) . . ?
C10 N4 Cu1 122.51(19) . . ?
O1 C2 N1 128.1(3) . . ?
O1 C2 C3 119.5(3) . . ?
N1 C2 C3 112.4(2) . . ?
N2 C3 C4 120.3(3) . . ?
N2 C3 C2 112.4(2) . . ?
C4 C3 C2 127.3(3) . . ?
C3 C4 C5 117.9(3) . . ?
C6 C5 C4 120.4(3) . . ?
C7 C6 C5 118.3(3) . . ?
N2 C7 C6 120.1(3) . . ?
N2 C7 C8 111.8(3) . . ?
C6 C7 C8 128.0(3) . . ?
O2 C8 N3 128.5(3) . . ?
O2 C8 C7 118.6(3) . . ?
N3 C8 C7 112.9(2) . . ?
N4 C10 C11 122.7(3) . . ?
C10 C11 C12 119.1(3) . . ?
C11 C12 C13 119.0(3) . . ?
C14 C13 C12 118.7(3) . . ?
N4 C14 C13 122.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.923(2) . ?
Cu1 N4 1.982(2) . ?
Cu1 N1 1.989(2) . ?
Cu1 N3 2.008(2) . ?
O1 C2 1.249(4) . ?
O2 C8 1.256(3) . ?
N1 C2 1.333(4) . ?
N1 C1 1.462(4) . ?
N2 C3 1.333(4) . ?
N2 C7 1.335(4) . ?
N3 C8 1.323(4) . ?
N3 C9 1.460(4) . ?
N4 C14 1.348(4) . ?
N4 C10 1.348(4) . ?
C2 C3 1.515(4) . ?
C3 C4 1.376(4) . ?
C4 C5 1.398(4) . ?
C5 C6 1.394(4) . ?
C6 C7 1.372(4) . ?
C7 C8 1.514(4) . ?
C10 C11 1.370(4) . ?
C11 C12 1.380(4) . ?
C12 C13 1.387(5) . ?
C13 C14 1.376(4) . ?
