#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/07/4320762.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_4320762
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            'C24 H15.5 Cl Cu N6.5 Na O6'
_chemical_formula_weight         612.91
_chemical_name_common            '[Cu(dmppy)(o-phen)][NaClO4].1.5CH3CN'
_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                 96.201(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.546(2)
_cell_length_b                   10.741(2)
_cell_length_c                   21.402(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      3.3
_cell_volume                     2638.7(8)
_computing_cell_refinement       'Siemens P3-PC'
_computing_data_collection       'Siemens P3-PC'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL 6.1 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL 6.1 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Siemens P3'
_diffrn_measurement_method       ω
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5936
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  0.9244
_exptl_absorpt_correction_T_min  0.6459
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2, Parkin, S., Moezzi, B. and Hope, H. J. Appl. Crystallogr. 28 
(1995) 53-56.
;
_exptl_crystal_colour            'teal blue'
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0904P)²+6.3714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.2035
_reflns_number_gt                3775
_reflns_number_total             5936
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic010523n_6.cif
_cod_data_source_block           mn1214
_cod_original_cell_volume        2638.4(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C24 H15.50 Cl Cu N6.50 Na O6'
_cod_database_code               4320762
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 0.34329(5) 0.04576(6) 1.07791(3) 0.02143(19) Uani 1 1 d . . .
O1 O 0.3167(4) -0.2499(4) 0.95950(19) 0.0314(9) Uani 1 1 d . . .
O2 O 0.4325(4) 0.3827(4) 1.0089(2) 0.0388(11) Uani 1 1 d . . .
N1 N 0.3343(4) -0.1313(4) 1.0502(2) 0.0257(10) Uani 1 1 d . . .
N2 N 0.3613(4) 0.0666(4) 0.99014(19) 0.0196(9) Uani 1 1 d . . .
N3 N 0.3930(4) 0.2242(5) 1.0773(2) 0.0283(10) Uani 1 1 d . . .
N4 N 0.1553(4) 0.0941(4) 1.0807(2) 0.0231(9) Uani 1 1 d . . .
N5 N 0.3258(4) 0.0292(4) 1.1714(2) 0.0225(9) Uani 1 1 d . . .
C1 C 0.3224(6) -0.2422(6) 1.0889(3) 0.0362(15) Uani 1 1 d . . .
C2 C 0.3309(5) -0.1487(5) 0.9886(3) 0.0233(11) Uani 1 1 d . . .
C3 C 0.3427(4) -0.0315(5) 0.9527(3) 0.0232(11) Uani 1 1 d . . .
C4 C 0.3355(5) -0.0175(6) 0.8880(3) 0.0291(13) Uani 1 1 d . . .
H4 H 0.3236 -0.0872 0.8607 0.035 Uiso 1 1 calc R . .
C5 C 0.3463(5) 0.1028(6) 0.8644(3) 0.0295(13) Uani 1 1 d . . .
H5 H 0.3392 0.1158 0.8202 0.035 Uiso 1 1 calc R . .
C6 C 0.3675(5) 0.2047(6) 0.9050(3) 0.0305(13) Uani 1 1 d . . .
H6 H 0.3757 0.2865 0.8892 0.037 Uiso 1 1 calc R . .
C7 C 0.3760(4) 0.1818(5) 0.9691(2) 0.0226(11) Uani 1 1 d . . .
C8 C 0.4012(5) 0.2730(5) 1.0220(3) 0.0255(12) Uani 1 1 d . . .
C9 C 0.4148(6) 0.3070(7) 1.1314(3) 0.0421(16) Uani 1 1 d . . .
C10 C 0.1310(4) 0.0995(5) 1.1405(3) 0.0227(11) Uani 1 1 d . . .
C11 C 0.2207(5) 0.0617(5) 1.1889(3) 0.0248(11) Uani 1 1 d . . .
C12 C 0.0748(5) 0.1305(6) 1.0357(3) 0.0301(13) Uani 1 1 d . . .
H12 H 0.0921 0.1283 0.9933 0.036 Uiso 1 1 calc R . .
C13 C -0.0357(5) 0.1726(6) 1.0486(3) 0.0334(14) Uani 1 1 d . . .
H13 H -0.0921 0.1966 1.0151 0.040 Uiso 1 1 calc R . .
C14 C -0.0615(5) 0.1788(5) 1.1087(3) 0.0291(13) Uani 1 1 d . . .
H14 H -0.1352 0.2089 1.1178 0.035 Uiso 1 1 calc R . .
C15 C 0.0219(5) 0.1401(5) 1.1576(3) 0.0260(12) Uani 1 1 d . . .
C16 C 0.0017(5) 0.1385(6) 1.2222(3) 0.0317(13) Uani 1 1 d . . .
H16 H -0.0713 0.1660 1.2336 0.038 Uiso 1 1 calc R . .
C17 C 0.0834(5) 0.0991(6) 1.2674(3) 0.0314(13) Uani 1 1 d . . .
H17 H 0.0662 0.0954 1.3098 0.038 Uiso 1 1 calc R . .
C18 C 0.1972(5) 0.0623(5) 1.2519(3) 0.0295(13) Uani 1 1 d . . .
C19 C 0.2883(5) 0.0257(6) 1.2977(3) 0.0346(14) Uani 1 1 d . . .
H19 H 0.2763 0.0244 1.3409 0.042 Uiso 1 1 calc R . .
C20 C 0.3948(5) -0.0080(6) 1.2793(3) 0.0366(15) Uani 1 1 d . . .
H20 H 0.4566 -0.0338 1.3095 0.044 Uiso 1 1 calc R . .
C21 C 0.4100(5) -0.0035(6) 1.2155(3) 0.0331(14) Uani 1 1 d . . .
H21 H 0.4840 -0.0249 1.2031 0.040 Uiso 1 1 calc R . .
N6 N 0.0226(8) -0.2414(10) 1.1017(4) 0.099(3) Uani 1 1 d . . .
C22 C -0.0119(7) -0.2208(7) 1.1470(4) 0.0479(18) Uani 1 1 d . . .
C23 C -0.0587(7) -0.1949(8) 1.2045(4) 0.056(2) Uani 1 1 d . . .
H23A H -0.1118 -0.2620 1.2137 0.067 Uiso 1 1 calc R . .
H23B H -0.1015 -0.1159 1.2007 0.067 Uiso 1 1 calc R . .
H23C H 0.0048 -0.1888 1.2386 0.067 Uiso 1 1 calc R . .
N7 N 0.1818(11) 0.4897(12) 1.0237(6) 0.050(3) Uani 0.50 1 d P . .
C24 C 0.0646(10) 0.4963(9) 1.0086(4) 0.075(3) Uani 1 1 d . . .
Cl1 Cl 0.24224(11) 0.52927(13) 0.81955(6) 0.0277(3) Uani 1 1 d . . .
O3 O 0.1677(6) 0.5111(7) 0.8673(3) 0.0753(19) Uani 1 1 d . . .
O4 O 0.2321(5) 0.6530(5) 0.7965(2) 0.0565(15) Uani 1 1 d . . .
O5 O 0.3593(4) 0.5086(5) 0.8458(3) 0.0542(14) Uani 1 1 d . . .
O6 O 0.2154(5) 0.4434(5) 0.7692(2) 0.0534(13) Uani 1 1 d . . .
Na1 Na 0.3727(2) 0.5540(2) 0.95825(14) 0.0475(7) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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 N1 80.09(19) . . ?
N2 Cu1 N3 79.66(19) . . ?
N1 Cu1 N3 156.7(2) . . ?
N2 Cu1 N5 178.24(19) . . ?
N1 Cu1 N5 101.62(19) . . ?
N3 Cu1 N5 98.58(19) . . ?
N2 Cu1 N4 101.91(17) . . ?
N1 Cu1 N4 102.11(18) . . ?
N3 Cu1 N4 93.30(18) . . ?
N5 Cu1 N4 78.17(17) . . ?
C2 O1 Na1 144.2(4) . 1_545 ?
C8 O2 Na1 143.1(4) . . ?
C8 O2 Na1 118.7(4) . 3_667 ?
Na1 O2 Na1 98.15(17) . 3_667 ?
C2 N1 C1 116.9(5) . . ?
C2 N1 Cu1 115.2(4) . . ?
C1 N1 Cu1 127.8(4) . . ?
C3 N2 C7 123.4(5) . . ?
C3 N2 Cu1 118.0(4) . . ?
C7 N2 Cu1 117.9(4) . . ?
C8 N3 C9 116.8(5) . . ?
C8 N3 Cu1 116.1(4) . . ?
C9 N3 Cu1 127.1(4) . . ?
C12 N4 C10 118.6(5) . . ?
C12 N4 Cu1 131.0(4) . . ?
C10 N4 Cu1 109.8(3) . . ?
C21 N5 C11 118.8(5) . . ?
C21 N5 Cu1 125.3(4) . . ?
C11 N5 Cu1 115.8(4) . . ?
O1 C2 N1 127.1(5) . . ?
O1 C2 C3 119.4(5) . . ?
N1 C2 C3 113.5(5) . . ?
N2 C3 C4 120.3(5) . . ?
N2 C3 C2 112.2(5) . . ?
C4 C3 C2 127.5(5) . . ?
C3 C4 C5 117.6(5) . . ?
C4 C5 C6 120.9(5) . . ?
C7 C6 C5 117.6(5) . . ?
N2 C7 C6 120.1(5) . . ?
N2 C7 C8 111.8(5) . . ?
C6 C7 C8 128.1(5) . . ?
O2 C8 N3 128.4(5) . . ?
O2 C8 C7 118.3(5) . . ?
N3 C8 C7 113.2(5) . . ?
N4 C10 C15 122.9(5) . . ?
N4 C10 C11 117.7(5) . . ?
C15 C10 C11 119.4(5) . . ?
N5 C11 C18 122.6(5) . . ?
N5 C11 C10 118.1(5) . . ?
C18 C11 C10 119.3(5) . . ?
N4 C12 C13 122.2(6) . . ?
C14 C13 C12 119.9(6) . . ?
C13 C14 C15 119.3(5) . . ?
C14 C15 C10 117.1(5) . . ?
C14 C15 C16 123.7(5) . . ?
C10 C15 C16 119.2(5) . . ?
C17 C16 C15 121.7(5) . . ?
C16 C17 C18 120.4(5) . . ?
C11 C18 C19 117.2(5) . . ?
C11 C18 C17 119.8(5) . . ?
C19 C18 C17 123.0(6) . . ?
C20 C19 C18 119.6(6) . . ?
C19 C20 C21 118.7(6) . . ?
N5 C21 C20 123.0(6) . . ?
N6 C22 C23 178.7(10) . . ?
C24 N7 Na1 132.9(9) . . ?
N7 C24 C24 179.5(13) . 3_567 ?
O4 Cl1 O3 110.2(4) . . ?
O4 Cl1 O5 108.9(4) . . ?
O3 Cl1 O5 108.5(4) . . ?
O4 Cl1 O6 109.9(3) . . ?
O3 Cl1 O6 110.8(4) . . ?
O5 Cl1 O6 108.5(3) . . ?
O4 Cl1 Na1 105.0(2) . . ?
O3 Cl1 Na1 66.7(3) . . ?
O5 Cl1 Na1 46.6(2) . . ?
O6 Cl1 Na1 143.0(2) . . ?
Cl1 O3 Na1 87.0(3) . . ?
Cl1 O5 Na1 108.3(3) . . ?
O1 Na1 O2 150.1(2) 1_565 . ?
O1 Na1 O2 89.56(18) 1_565 3_667 ?
O2 Na1 O2 81.85(17) . 3_667 ?
O1 Na1 O5 102.42(19) 1_565 . ?
O2 Na1 O5 107.5(2) . . ?
O2 Na1 O5 107.8(2) 3_667 . ?
O1 Na1 N7 88.9(3) 1_565 . ?
O2 Na1 N7 76.8(3) . . ?
O2 Na1 N7 133.4(3) 3_667 . ?
O5 Na1 N7 118.0(3) . . ?
O1 Na1 O3 86.63(19) 1_565 . ?
O2 Na1 O3 112.4(2) . . ?
O2 Na1 O3 155.4(2) 3_667 . ?
O5 Na1 O3 49.79(16) . . ?
N7 Na1 O3 70.9(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 1.925(4) . ?
Cu1 N1 1.992(5) . ?
Cu1 N3 2.001(5) . ?
Cu1 N5 2.041(4) . ?
Cu1 N4 2.239(4) . ?
O1 C2 1.255(7) . ?
O1 Na1 2.204(5) 1_545 ?
O2 C8 1.273(7) . ?
O2 Na1 2.207(5) . ?
O2 Na1 2.382(5) 3_667 ?
N1 C2 1.327(7) . ?
N1 C1 1.466(7) . ?
N2 C3 1.327(7) . ?
N2 C7 1.334(7) . ?
N3 C8 1.306(7) . ?
N3 C9 1.461(7) . ?
N4 C12 1.323(7) . ?
N4 C10 1.341(7) . ?
N5 C21 1.327(7) . ?
N5 C11 1.353(7) . ?
C2 C3 1.488(8) . ?
C3 C4 1.387(8) . ?
C4 C5 1.398(8) . ?
C5 C6 1.403(8) . ?
C6 C7 1.386(7) . ?
C7 C8 1.502(8) . ?
C10 C15 1.418(7) . ?
C10 C11 1.442(7) . ?
C11 C18 1.405(8) . ?
C12 C13 1.409(8) . ?
C13 C14 1.353(9) . ?
C14 C15 1.406(8) . ?
C15 C16 1.428(8) . ?
C16 C17 1.344(9) . ?
C17 C18 1.444(8) . ?
C18 C19 1.414(8) . ?
C19 C20 1.379(9) . ?
C20 C21 1.396(8) . ?
N6 C22 1.109(10) . ?
C22 C23 1.424(10) . ?
N7 C24 1.357(16) . ?
N7 Na1 2.822(12) . ?
C24 C24 1.50(2) 3_567 ?
Cl1 O4 1.418(5) . ?
Cl1 O3 1.418(5) . ?
Cl1 O5 1.424(5) . ?
Cl1 O6 1.427(5) . ?
Cl1 Na1 3.192(3) . ?
O3 Na1 2.935(7) . ?
O5 Na1 2.443(6) . ?
Na1 O1 2.204(5) 1_565 ?
Na1 O2 2.382(5) 3_667 ?
