#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:29:59 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179063 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/25/4302547.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_4302547
loop_
_publ_author_name
'Vadapalli Chandrasekhar'
'Tapas Senapati'
'E. Carolina Sañudo'
'R. Clérac'
_publ_contact_author_address
;Head, Department of Chemistry
Indian Institute of Technology Kanpur
Kanpur 208016
Uttarpradesh
India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91-512-259 7436'
_publ_contact_author_name        'Prof. V. Chandrasekhar'
_publ_contact_author_phone       '+91-512-259 7259'
_publ_section_title
;
Tri-, Tetra-, and Hexanuclear Copper(II) Phosphonates Containing N-Donor
Chelating Ligands: Synthesis, Structure, Magnetic Properties, and Nuclease
Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6192
_journal_page_last               6204
_journal_paper_doi               10.1021/ic900522u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C50 H54 Cl2 Cu4 N12 O6 P2, 4(CH4O), 2(Cl)'
_chemical_formula_sum            'C54 H70 Cl4 Cu4 N12 O10 P2'
_chemical_formula_weight         1505.12
_chemical_melting_point          280
_chemical_name_common            Copperphosphonate
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.858(5)
_cell_angle_beta                 105.855(5)
_cell_angle_gamma                95.954(5)
_cell_formula_units_Z            1
_cell_length_a                   9.736(5)
_cell_length_b                   12.313(5)
_cell_length_c                   14.588(5)
_cell_measurement_reflns_used    948
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.52
_cell_measurement_theta_min      2.26
_cell_volume                     1606.3(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.1135
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9128
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  0.8930
_exptl_absorpt_correction_T_min  0.7743
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1083P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.2142
_reflns_number_gt                3974
_reflns_number_total             6173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900522u_si_001_2.cif
_cod_data_source_block           Complex-3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4302547
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.51413(10) 0.78911(7) -0.04514(6) 0.0287(3) Uani 1 1 d . . .
Cu2 Cu 0.75120(9) 1.00821(7) 0.12550(6) 0.0292(3) Uani 1 1 d . . .
Cl1 Cl 0.7965(2) 0.81486(16) 0.02751(14) 0.0372(5) Uani 1 1 d . . .
Cl2 Cl 0.9074(3) 0.3481(2) 0.55515(17) 0.0683(7) Uani 1 1 d . . .
P1 P 0.5847(2) 1.02227(14) -0.08753(13) 0.0242(4) Uani 1 1 d . . .
O1 O 0.5415(5) 0.9114(4) 0.0812(3) 0.0247(10) Uani 1 1 d . . .
O2 O 0.7058(5) 1.0637(4) 0.0106(3) 0.0339(12) Uani 1 1 d . . .
O3 O 0.5232(5) 0.8957(4) -0.1238(3) 0.0316(12) Uani 1 1 d . . .
O4 O 0.6028(14) 0.3640(11) 0.5953(9) 0.147(4) Uani 1 1 d . . .
H4 H 0.6777 0.3635 0.5799 0.220 Uiso 1 1 calc R . .
O5 O 1.0424(7) 0.3718(6) 0.7759(5) 0.067(2) Uani 1 1 d . . .
H5 H 1.0026 0.3755 0.7197 0.100 Uiso 1 1 calc R . .
N1 N 0.4659(7) 0.6692(5) -0.1745(4) 0.0341(15) Uani 1 1 d . . .
N2 N 0.2790(7) 0.5613(6) -0.1446(5) 0.0432(18) Uani 1 1 d . . .
N3 N 0.4363(7) 0.6721(5) 0.0117(4) 0.0323(14) Uani 1 1 d . . .
N4 N 0.8026(6) 0.9769(5) 0.2585(4) 0.0311(14) Uani 1 1 d . . .
N5 N 0.8438(7) 1.1740(5) 0.3393(4) 0.0391(16) Uani 1 1 d . . .
H1N H 0.8104 1.2213 0.3776 0.047 Uiso 1 1 calc R . .
N6 N 0.9008(6) 1.1545(5) 0.1901(4) 0.0305(14) Uani 1 1 d . . .
C1 C 0.6619(8) 1.0595(6) -0.1768(5) 0.0309(17) Uani 1 1 d . . .
H1 H 0.6926 1.1423 -0.1568 0.037 Uiso 1 1 calc R . .
C2 C 0.5586(9) 1.0229(8) -0.2854(6) 0.049(2) Uani 1 1 d . . .
H2A H 0.4966 0.9501 -0.2998 0.059 Uiso 1 1 calc R . .
H2B H 0.4983 1.0792 -0.2973 0.059 Uiso 1 1 calc R . .
C3 C 0.6600(11) 1.0147(10) -0.3474(6) 0.065(3) Uani 1 1 d . . .
H3A H 0.6111 0.9664 -0.4143 0.078 Uiso 1 1 calc R . .
H3B H 0.6972 1.0894 -0.3509 0.078 Uiso 1 1 calc R . .
C4 C 0.7794(11) 0.9640(10) -0.2948(8) 0.078(3) Uani 1 1 d . . .
H4A H 0.8692 0.9889 -0.3068 0.093 Uiso 1 1 calc R . .
H4B H 0.7557 0.8817 -0.3184 0.093 Uiso 1 1 calc R . .
C5 C 0.7965(8) 1.0043(7) -0.1829(6) 0.042(2) Uani 1 1 d . . .
H5A H 0.8854 1.0592 -0.1476 0.050 Uiso 1 1 calc R . .
H5B H 0.7983 0.9405 -0.1547 0.050 Uiso 1 1 calc R . .
C6 C 0.8044(8) 0.8704(7) 0.2675(6) 0.0397(19) Uani 1 1 d . . .
H6 H 0.8023 0.8129 0.2123 0.048 Uiso 1 1 calc R . .
C7 C 0.8091(9) 0.8429(7) 0.3534(6) 0.046(2) Uani 1 1 d . . .
H7 H 0.8100 0.7683 0.3563 0.055 Uiso 1 1 calc R . .
C8 C 0.8123(9) 0.9264(7) 0.4351(6) 0.047(2) Uani 1 1 d . . .
H8 H 0.8107 0.9088 0.4933 0.056 Uiso 1 1 calc R . .
C9 C 0.8181(9) 1.0369(8) 0.4303(5) 0.046(2) Uani 1 1 d . . .
H9 H 0.8203 1.0949 0.4852 0.055 Uiso 1 1 calc R . .
C10 C 0.8208(8) 1.0608(7) 0.3415(5) 0.0363(18) Uani 1 1 d . . .
C11 C 0.9135(7) 1.2176(6) 0.2827(5) 0.0292(16) Uani 1 1 d . . .
C12 C 0.9977(9) 1.3282(6) 0.3206(6) 0.043(2) Uani 1 1 d . . .
H12 H 1.0033 1.3733 0.3830 0.051 Uiso 1 1 calc R . .
C13 C 1.0703(10) 1.3679(7) 0.2645(7) 0.055(2) Uani 1 1 d . . .
H13 H 1.1274 1.4402 0.2895 0.066 Uiso 1 1 calc R . .
C14 C 1.0605(9) 1.3021(7) 0.1704(6) 0.047(2) Uani 1 1 d . . .
H14 H 1.1097 1.3284 0.1314 0.057 Uiso 1 1 calc R . .
C15 C 0.9725(8) 1.1938(7) 0.1371(6) 0.0368(18) Uani 1 1 d . . .
H15 H 0.9647 1.1478 0.0746 0.044 Uiso 1 1 calc R . .
C16 C 0.5419(10) 0.6847(7) -0.2375(6) 0.047(2) Uani 1 1 d . . .
H16 H 0.6260 0.7395 -0.2128 0.057 Uiso 1 1 calc R . .
C17 C 0.5005(12) 0.6233(8) -0.3357(6) 0.061(3) Uani 1 1 d . . .
H17 H 0.5555 0.6326 -0.3772 0.073 Uiso 1 1 calc R . .
C18 C 0.3626(12) 0.5418(8) -0.3704(7) 0.063(3) Uani 1 1 d . . .
H18 H 0.3252 0.5010 -0.4370 0.076 Uiso 1 1 calc R . .
C19 C 0.2926(10) 0.5261(7) -0.3088(6) 0.049(2) Uani 1 1 d . . .
H19 H 0.2060 0.4740 -0.3321 0.059 Uiso 1 1 calc R . .
C20 C 0.3454(8) 0.5863(6) -0.2087(5) 0.0318(17) Uani 1 1 d . . .
C21 C 0.3340(8) 0.5799(6) -0.0426(5) 0.0319(17) Uani 1 1 d . . .
C22 C 0.2781(9) 0.5013(7) 0.0012(7) 0.047(2) Uani 1 1 d . . .
H22 H 0.2061 0.4389 -0.0374 0.056 Uiso 1 1 calc R . .
C23 C 0.3317(11) 0.5196(8) 0.0996(7) 0.057(3) Uani 1 1 d . . .
H23 H 0.2970 0.4692 0.1299 0.068 Uiso 1 1 calc R . .
C24 C 0.4413(9) 0.6153(7) 0.1578(7) 0.046(2) Uani 1 1 d . . .
H24 H 0.4795 0.6288 0.2261 0.056 Uiso 1 1 calc R . .
C25 C 0.4879(9) 0.6857(6) 0.1107(5) 0.0390(19) Uani 1 1 d . . .
H25 H 0.5605 0.7481 0.1486 0.047 Uiso 1 1 calc R . .
C27 C 0.9428(12) 0.3347(13) 0.8135(9) 0.104(5) Uani 1 1 d . . .
H27A H 0.9682 0.2702 0.8360 0.156 Uiso 1 1 calc R . .
H27B H 0.8498 0.3129 0.7633 0.156 Uiso 1 1 calc R . .
H27C H 0.9386 0.3942 0.8683 0.156 Uiso 1 1 calc R . .
C28 C 0.5167(18) 0.2631(13) 0.5522(13) 0.136(7) Uani 1 1 d . . .
H29A H 0.5085 0.2262 0.6019 0.204 Uiso 1 1 calc R . .
H29B H 0.5570 0.2172 0.5067 0.204 Uiso 1 1 calc R . .
H29C H 0.4223 0.2730 0.5166 0.204 Uiso 1 1 calc R . .
H2N H 0.216(9) 0.500(7) -0.164(6) 0.05(3) Uiso 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'
P P 0.1023 0.0942 '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'
Cu Cu 0.3201 1.2651 '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
O3 Cu1 N1 84.9(2) . . ?
O3 Cu1 N3 161.4(2) . . ?
N1 Cu1 N3 88.7(2) . . ?
O3 Cu1 O1 94.26(18) . . ?
N1 Cu1 O1 174.2(2) . . ?
N3 Cu1 O1 90.4(2) . . ?
O3 Cu1 Cl1 93.85(15) . . ?
N1 Cu1 Cl1 103.82(19) . . ?
N3 Cu1 Cl1 104.62(18) . . ?
O1 Cu1 Cl1 81.90(13) . . ?
O2 Cu2 N4 170.6(2) . . ?
O2 Cu2 N6 85.1(2) . . ?
N4 Cu2 N6 87.5(2) . . ?
O2 Cu2 O1 91.79(19) . . ?
N4 Cu2 O1 92.3(2) . . ?
N6 Cu2 O1 153.8(2) . . ?
O2 Cu2 Cl1 92.96(16) . . ?
N4 Cu2 Cl1 96.10(18) . . ?
N6 Cu2 Cl1 125.68(18) . . ?
O1 Cu2 Cl1 80.41(13) . . ?
Cu2 Cl1 Cu1 79.33(6) . . ?
O2 P1 O3 116.6(3) . . ?
O2 P1 O1 109.2(3) . 2_675 ?
O3 P1 O1 108.8(3) . 2_675 ?
O2 P1 C1 105.2(3) . . ?
O3 P1 C1 108.4(3) . . ?
O1 P1 C1 108.5(3) 2_675 . ?
P1 O1 Cu1 117.8(3) 2_675 . ?
P1 O1 Cu2 117.0(2) 2_675 . ?
Cu1 O1 Cu2 108.5(2) . . ?
P1 O2 Cu2 132.0(3) . . ?
P1 O3 Cu1 128.3(3) . . ?
C20 N1 C16 118.9(7) . . ?
C20 N1 Cu1 122.6(5) . . ?
C16 N1 Cu1 117.4(5) . . ?
C20 N2 C21 129.5(7) . . ?
C21 N3 C25 117.2(6) . . ?
C21 N3 Cu1 123.9(5) . . ?
C25 N3 Cu1 118.9(5) . . ?
C10 N4 C6 117.3(6) . . ?
C10 N4 Cu2 120.4(5) . . ?
C6 N4 Cu2 121.9(5) . . ?
C11 N5 C10 127.0(6) . . ?
C15 N6 C11 120.0(6) . . ?
C15 N6 Cu2 119.3(5) . . ?
C11 N6 Cu2 120.2(5) . . ?
C5 C1 C2 104.5(6) . . ?
C5 C1 P1 112.4(5) . . ?
C2 C1 P1 115.1(5) . . ?
C3 C2 C1 103.9(7) . . ?
C4 C3 C2 104.3(8) . . ?
C3 C4 C5 107.4(8) . . ?
C4 C5 C1 105.1(6) . . ?
N4 C6 C7 123.3(7) . . ?
C8 C7 C6 119.0(8) . . ?
C7 C8 C9 119.3(8) . . ?
C8 C9 C10 119.0(8) . . ?
N4 C10 N5 119.4(7) . . ?
N4 C10 C9 121.3(7) . . ?
N5 C10 C9 119.4(7) . . ?
N6 C11 N5 119.7(6) . . ?
N6 C11 C12 120.2(7) . . ?
N5 C11 C12 120.2(7) . . ?
C13 C12 C11 119.0(7) . . ?
C12 C13 C14 120.9(8) . . ?
C13 C14 C15 116.7(8) . . ?
N6 C15 C14 123.1(7) . . ?
N1 C16 C17 123.3(9) . . ?
C16 C17 C18 115.2(9) . . ?
C19 C18 C17 120.8(8) . . ?
C18 C19 C20 121.0(9) . . ?
N2 C20 N1 119.5(7) . . ?
N2 C20 C19 120.1(7) . . ?
N1 C20 C19 120.5(8) . . ?
N3 C21 N2 119.4(7) . . ?
N3 C21 C22 122.1(7) . . ?
N2 C21 C22 118.5(7) . . ?
C23 C22 C21 118.2(8) . . ?
C22 C23 C24 120.4(8) . . ?
C25 C24 C23 117.6(8) . . ?
C24 C25 N3 124.4(7) . . ?
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 O3 1.949(5) . ?
Cu1 N1 1.999(6) . ?
Cu1 N3 2.008(6) . ?
Cu1 O1 2.014(4) . ?
Cu1 Cl1 2.617(2) . ?
Cu2 O2 1.917(5) . ?
Cu2 N4 2.008(6) . ?
Cu2 N6 2.036(5) . ?
Cu2 O1 2.100(4) . ?
Cu2 Cl1 2.615(2) . ?
P1 O2 1.518(5) . ?
P1 O3 1.518(5) . ?
P1 O1 1.555(5) 2_675 ?
P1 C1 1.796(7) . ?
O1 P1 1.555(5) 2_675 ?
O4 C28 1.327(15) . ?
O5 C27 1.330(13) . ?
N1 C20 1.362(9) . ?
N1 C16 1.362(10) . ?
N2 C20 1.348(10) . ?
N2 C21 1.389(10) . ?
N3 C21 1.345(9) . ?
N3 C25 1.354(9) . ?
N4 C10 1.345(9) . ?
N4 C6 1.350(9) . ?
N5 C11 1.369(9) . ?
N5 C10 1.398(10) . ?
N6 C15 1.313(9) . ?
N6 C11 1.352(9) . ?
C1 C5 1.551(10) . ?
C1 C2 1.555(10) . ?
C2 C3 1.506(12) . ?
C3 C4 1.491(14) . ?
C4 C5 1.544(12) . ?
C6 C7 1.365(11) . ?
C7 C8 1.365(12) . ?
C8 C9 1.374(12) . ?
C9 C10 1.402(11) . ?
C11 C12 1.412(10) . ?
C12 C13 1.358(12) . ?
C13 C14 1.389(12) . ?
C14 C15 1.404(10) . ?
C16 C17 1.374(11) . ?
C17 C18 1.473(14) . ?
C18 C19 1.304(13) . ?
C19 C20 1.392(10) . ?
C21 C22 1.421(10) . ?
C22 C23 1.339(12) . ?
C23 C24 1.419(12) . ?
C24 C25 1.343(10) . ?
