#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:43:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179986 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/80/7028001.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7028001
loop_
_publ_author_name
'Manikandan, Palanichamy'
'Subramoni, Mahadevan'
'Varghese, Babu'
'ThangiahManoharan, Periakaruppan'
_publ_section_title
;
 Ligand dynamics in tetracoordinate copper(I) complexes of
 bis(pyrazolyl)pyridine ligands †
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3219
_journal_paper_doi               10.1039/a801622d
_journal_year                    1998
_chemical_formula_sum            'C60 H66 Cl2 Cu2 N10 O8 P2'
_chemical_formula_weight         1315.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.769(3)
_cell_length_b                   14.386(2)
_cell_length_c                   20.284(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      12
_cell_volume                     6817.3(18)
_computing_cell_refinement       'CAD4 Programs'
_computing_data_collection       'CAD4 Programs'
_computing_data_reduction        MolEN
_computing_molecular_graphics    ZORTEP
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'CAD4 Diffractometer'
_diffrn_measurement_method       'omega twotheta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-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    0.0121
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3734
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  'one hour'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'faint yellow'
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       plate
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00000(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.122
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         3734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_obs          0.0466
_refine_ls_shift/esd_max         -1.048
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0737P)²+18.8900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1344
_refine_ls_wR_factor_obs         0.1344
_reflns_number_observed          3734
_reflns_number_total             3734
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            d801622sup1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'psi scan'
changed to 'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+18.8900P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+18.8900P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6817.3(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7028001
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cu Cu 0.14636(3) 0.07703(4) 0.00084(3) 0.0531(2) Uani 1 d .
Cl Cl 0.13802(10) -0.40835(15) -0.13006(12) 0.1020(6) Uani 1 d .
P P 0.19172(5) 0.15516(9) -0.06772(6) 0.0493(3) Uani 1 d .
O1 O 0.1059(4) -0.3873(7) -0.0829(4) 0.192(3) Uani 1 d .
O2 O 0.1717(6) -0.3338(10) -0.1337(9) 0.327(8) Uani 1 d .
O3 O 0.1041(6) -0.4079(10) -0.1946(6) 0.266(6) Uani 1 d .
O4 O 0.1672(4) -0.4882(6) -0.1197(5) 0.200(4) Uani 1 d .
N1 N 0.1720(2) -0.0522(3) 0.0459(2) 0.0479(9) Uani 1 d .
N2 N 0.0825(2) -0.0733(3) -0.0807(2) 0.0543(10) Uani 1 d .
N3 N 0.0741(2) 0.0121(3) -0.0546(2) 0.0525(10) Uani 1 d .
N4 N 0.1683(2) 0.1015(3) 0.1494(2) 0.0574(11) Uani 1 d .
N5 N 0.1424(2) 0.1409(3) 0.0903(2) 0.0609(11) Uani 1 d .
C1 C 0.1553(2) -0.1304(3) 0.0120(2) 0.0536(12) Uani 1 d .
C2 C 0.1535(3) -0.2160(4) 0.0425(3) 0.073(2) Uani 1 d .
H2 H 0.1422(3) -0.2693(4) 0.0176(3) 0.088 Uiso 1 calc R
C3 C 0.1693(3) -0.2195(4) 0.1121(3) 0.092(2) Uani 1 d .
H3 H 0.1688(3) -0.2756(4) 0.1348(3) 0.111 Uiso 1 calc R
C4 C 0.1855(3) -0.1405(4) 0.1462(3) 0.080(2) Uani 1 d .
H4 H 0.1955(3) -0.1424(4) 0.1927(3) 0.096 Uiso 1 calc R
C5 C 0.1874(2) -0.0574(4) 0.1137(2) 0.0562(12) Uani 1 d .
C6 C 0.1379(2) -0.1179(4) -0.0627(2) 0.0570(12) Uani 1 d .
H6A H 0.1664(2) -0.0806(4) -0.0790(2) 0.068 Uiso 1 calc R
H6B H 0.1365(2) -0.1782(4) -0.0844(2) 0.068 Uiso 1 calc R
C7 C 0.0341(2) -0.1050(4) -0.1201(2) 0.0601(13) Uani 1 d .
C8 C 0.0325(3) -0.1968(4) -0.1560(3) 0.085(2) Uani 1 d .
H8A H 0.0690(3) -0.2270(4) -0.1440(3) 0.127 Uiso 1 calc R
H8B H 0.0241(3) -0.1865(4) -0.2035(3) 0.127 Uiso 1 calc R
H8C H 0.0033(3) -0.2354(4) -0.1433(3) 0.127 Uiso 1 calc R
C9 C -0.0060(2) -0.0383(4) -0.1205(3) 0.0611(13) Uani 1 d .
H9 H -0.0436(2) -0.0402(4) -0.1435(3) 0.073 Uiso 1 calc R
C10 C 0.0195(2) 0.0334(4) -0.0802(2) 0.0549(12) Uani 1 d .
C11 C -0.0057(3) 0.1240(4) -0.0633(3) 0.073(2) Uani 1 d .
H11A H 0.0229(3) 0.1592(4) -0.0341(3) 0.110 Uiso 1 calc R
H11B H -0.0374(3) 0.1121(4) -0.0414(3) 0.110 Uiso 1 calc R
H11C H -0.0186(3) 0.1585(4) -0.1038(3) 0.110 Uiso 1 calc R
C12 C 0.2106(2) 0.0296(4) 0.1489(3) 0.0630(13) Uani 1 d .
H12A H 0.2275(2) 0.0144(4) 0.1948(3) 0.076 Uiso 1 calc R
H12B H 0.2407(2) 0.0537(4) 0.1273(3) 0.076 Uiso 1 calc R
C13 C 0.1601(3) 0.1536(4) 0.2027(3) 0.069(2) Uani 1 d .
C14 C 0.1871(4) 0.1309(5) 0.2734(3) 0.110(3) Uani 1 d .
H14A H 0.2086(4) 0.0742(5) 0.2741(3) 0.164 Uiso 1 calc R
H14B H 0.1578(4) 0.1234(5) 0.2998(3) 0.164 Uiso 1 calc R
H14C H 0.2123(4) 0.1805(5) 0.2916(3) 0.164 Uiso 1 calc R
C15 C 0.1265(3) 0.2259(4) 0.1775(3) 0.072(2) Uani 1 d .
H15 H 0.1126(3) 0.2724(4) 0.2020(3) 0.087 Uiso 1 calc R
C16 C 0.1164(2) 0.2173(4) 0.1072(3) 0.0614(13) Uani 1 d .
C17 C 0.0846(3) 0.2808(4) 0.0548(3) 0.086(2) Uani 1 d .
H17A H 0.0852(3) 0.2556(4) 0.0111(3) 0.129 Uiso 1 calc R
H17B H 0.1026(3) 0.3409(4) 0.0587(3) 0.129 Uiso 1 calc R
H17C H 0.0457(3) 0.2868(4) 0.0610(3) 0.129 Uiso 1 calc R
C18 C 0.2481(2) 0.0926(3) -0.0981(2) 0.0572(13) Uani 1 d .
C19 C 0.2778(3) 0.0254(4) -0.0585(3) 0.0700(15) Uani 1 d .
H19 H 0.2670(3) 0.0110(4) -0.0178(3) 0.084 Uiso 1 calc R
C20 C 0.3232(3) -0.0217(5) -0.0765(4) 0.098(2) Uani 1 d .
H20 H 0.3443(3) -0.0644(5) -0.0475(4) 0.117 Uiso 1 calc R
C21 C 0.3366(4) -0.0034(6) -0.1399(5) 0.105(3) Uani 1 d .
H21 H 0.3652(4) -0.0374(6) -0.1547(5) 0.126 Uiso 1 calc R
C22 C 0.3079(3) 0.0639(5) -0.1797(3) 0.085(2) Uani 1 d .
H22 H 0.3185(3) 0.0778(5) -0.2206(3) 0.103 Uiso 1 calc R
C23 C 0.2633(2) 0.1120(4) -0.1604(2) 0.0679(15) Uani 1 d .
H23 H 0.2434(2) 0.1569(4) -0.1885(2) 0.082 Uiso 1 calc R
C24 C 0.1456(2) 0.1950(4) -0.1453(2) 0.0557(12) Uani 1 d .
C25 C 0.1125(2) 0.1310(4) -0.1842(2) 0.0671(15) Uani 1 d .
H25 H 0.1137(2) 0.0689(4) -0.1711(2) 0.080 Uiso 1 calc R
C26 C 0.0771(3) 0.1583(6) -0.2432(3) 0.085(2) Uani 1 d .
H26 H 0.0557(3) 0.1143(6) -0.2706(3) 0.102 Uiso 1 calc R
C27 C 0.0737(3) 0.2496(6) -0.2609(3) 0.101(2) Uani 1 d .
H27 H 0.0498(3) 0.2680(6) -0.3004(3) 0.122 Uiso 1 calc R
C28 C 0.1048(3) 0.3138(5) -0.2214(3) 0.100(2) Uani 1 d .
H28 H 0.1021(3) 0.3761(5) -0.2337(3) 0.120 Uiso 1 calc R
C29 C 0.1400(3) 0.2882(4) -0.1643(3) 0.078(2) Uani 1 d .
H29 H 0.1607(3) 0.3332(4) -0.1372(3) 0.093 Uiso 1 calc R
C30 C 0.2294(2) 0.2613(3) -0.0334(2) 0.0536(12) Uani 1 d .
H30A H 0.2511(2) 0.2864(3) -0.0654(2) 0.064 Uiso 1 calc R
H30B H 0.2019(2) 0.3077(3) -0.0255(2) 0.064 Uiso 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N5 Cu N3 120.6(2) .
N5 Cu N1 93.9(2) .
N3 Cu N1 88.97(15) .
N5 Cu P 115.77(13) .
N3 Cu P 109.58(11) .
N1 Cu P 125.67(11) .
O4 Cl O2 113.2(8) .
O4 Cl O1 114.9(6) .
O2 Cl O1 106.1(8) .
O4 Cl O3 110.0(7) .
O2 Cl O3 101.0(9) .
O1 Cl O3 110.7(7) .
C18 P C24 103.1(2) .
C18 P C30 101.6(2) .
C24 P C30 103.8(2) .
C18 P Cu 115.9(2) .
C24 P Cu 114.4(2) .
C30 P Cu 116.3(2) .
C1 N1 C5 118.2(4) .
C1 N1 Cu 118.9(3) .
C5 N1 Cu 119.3(3) .
C7 N2 N3 111.2(4) .
C7 N2 C6 129.3(4) .
N3 N2 C6 119.4(4) .
C10 N3 N2 104.8(4) .
C10 N3 Cu 138.2(4) .
N2 N3 Cu 116.5(3) .
C13 N4 N5 111.3(5) .
C13 N4 C12 127.1(5) .
N5 N4 C12 119.5(4) .
C16 N5 N4 105.7(4) .
C16 N5 Cu 133.9(4) .
N4 N5 Cu 120.3(3) .
N1 C1 C2 123.2(5) .
N1 C1 C6 114.6(4) .
C2 C1 C6 122.1(5) .
C1 C2 C3 117.5(5) .
C4 C3 C2 119.1(5) .
C3 C4 C5 121.4(5) .
N1 C5 C4 120.5(5) .
N1 C5 C12 116.3(4) .
C4 C5 C12 122.9(5) .
N2 C6 C1 112.0(4) .
C9 C7 N2 106.7(5) .
C9 C7 C8 131.7(5) .
N2 C7 C8 121.6(5) .
C7 C9 C10 107.1(5) .
N3 C10 C9 110.2(5) .
N3 C10 C11 120.6(5) .
C9 C10 C11 129.2(5) .
N4 C12 C5 114.0(4) .
C15 C13 N4 106.5(5) .
C15 C13 C14 130.5(6) .
N4 C13 C14 123.0(6) .
C13 C15 C16 107.1(5) .
N5 C16 C15 109.3(5) .
N5 C16 C17 121.2(5) .
C15 C16 C17 129.5(5) .
C19 C18 C23 118.7(5) .
C19 C18 P 119.0(4) .
C23 C18 P 122.3(4) .
C18 C19 C20 122.4(6) .
C19 C20 C21 118.1(7) .
C22 C21 C20 120.2(7) .
C21 C22 C23 121.0(6) .
C22 C23 C18 119.5(6) .
C25 C24 C29 118.4(5) .
C25 C24 P 118.3(4) .
C29 C24 P 123.2(4) .
C24 C25 C26 120.0(6) .
C27 C26 C25 119.9(6) .
C28 C27 C26 120.2(6) .
C29 C28 C27 120.6(6) .
C28 C29 C24 120.8(6) .
C30 C30 P 110.0(4) 7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N5 2.052(4) .
Cu N3 2.091(4) .
Cu N1 2.111(4) .
Cu P 2.2163(14) .
Cl O4 1.338(8) .
Cl O2 1.349(13) .
Cl O1 1.363(8) .
Cl O3 1.406(12) .
P C18 1.814(6) .
P C24 1.837(5) .
P C30 1.841(4) .
N1 C1 1.340(6) .
N1 C5 1.360(6) .
N2 C7 1.353(6) .
N2 N3 1.367(5) .
N2 C6 1.448(6) .
N3 C10 1.341(6) .
N4 C13 1.357(6) .
N4 N5 1.366(6) .
N4 C12 1.444(7) .
N5 C16 1.337(7) .
C1 C2 1.383(7) .
C1 C6 1.506(6) .
C2 C3 1.393(8) .
C3 C4 1.349(9) .
C4 C5 1.369(7) .
C5 C12 1.495(7) .
C7 C9 1.351(7) .
C7 C8 1.505(8) .
C9 C10 1.384(7) .
C10 C11 1.500(8) .
C13 C15 1.354(8) .
C13 C14 1.496(8) .
C15 C16 1.407(8) .
C16 C17 1.496(8) .
C18 C19 1.368(7) .
C18 C23 1.404(7) .
C19 C20 1.379(9) .
C20 C21 1.406(11) .
C21 C22 1.362(10) .
C22 C23 1.383(9) .
C24 C25 1.363(7) .
C24 C29 1.393(8) .
C25 C26 1.388(8) .
C26 C27 1.360(10) .
C27 C28 1.351(9) .
C28 C29 1.349(8) .
C30 C30 1.552(9) 7
