#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:56:56 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179605 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/69/4506940.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_4506940
loop_
_publ_author_name
'Tripuramallu, Bharat Kumar'
'Mukherjee, Sandip'
'Das, Samar K.'
_publ_section_title
;
 Mechanistic Aspects for the Formation of Copper Dimer Bridged by
 Phosphonic Acid and Extending Its Dimensionality by Organic and Inorganic
 Linkers: Synthesis, Structural Characterization, Magnetic Properties, and
 Theoretical Studies
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5579
_journal_paper_doi               10.1021/cg3011162
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C40 H52 Cu2 N4 O20 P4'
_chemical_formula_sum            'C40 H52 Cu2 N4 O20 P4'
_chemical_formula_weight         1159.82
_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                99.406(2)
_cell_angle_beta                 92.522(2)
_cell_angle_gamma                97.815(2)
_cell_formula_units_Z            1
_cell_length_a                   7.4340(8)
_cell_length_b                   11.6079(13)
_cell_length_c                   13.8609(16)
_cell_measurement_reflns_used    6957
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.53
_cell_volume                     1166.4(2)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11326
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.134
_exptl_absorpt_correction_T_max  0.9148
_exptl_absorpt_correction_T_min  0.8050
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0508P)²+0.5142P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                3828
_reflns_number_total             4132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3011162_si_002.cif
_cod_data_source_block           compound-3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4506940
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
Cu1 Cu 0.22299(3) 0.54982(2) 0.870568(17) 0.03016(10) Uani 1 1 d .
P1 P 0.05878(7) 0.65731(5) 1.06700(4) 0.02814(14) Uani 1 1 d .
P2 P 0.04620(8) 1.05813(5) 0.64702(4) 0.03313(15) Uani 1 1 d .
O4 O 0.2059(2) 0.60809(14) 1.00850(10) 0.0341(3) Uani 1 1 d .
O2 O 0.0262(2) 0.42005(13) 0.86466(11) 0.0361(3) Uani 1 1 d .
O1 O 0.4608(4) 0.4484(2) 0.8906(2) 0.0552(6) Uani 1 1 d .
C11 C 0.3293(3) 0.6023(2) 0.68766(16) 0.0345(5) Uani 1 1 d .
C15 C 0.0420(3) 0.8663(2) 0.92474(16) 0.0366(5) Uani 1 1 d .
H15 H 0.0647 0.9042 0.9895 0.044 Uiso 1 1 calc R
C17 C 0.0710(3) 0.8708(2) 0.75243(16) 0.0365(5) Uani 1 1 d .
C13 C -0.1178(3) 0.6883(2) 0.98573(17) 0.0365(5) Uani 1 1 d .
H13A H -0.1914 0.6142 0.9566 0.044 Uiso 1 1 calc R
H13B H -0.1959 0.7354 1.0244 0.044 Uiso 1 1 calc R
C12 C 0.4143(3) 0.70116(19) 0.75725(16) 0.0343(5) Uani 1 1 d .
C18 C -0.0247(3) 0.7574(2) 0.73235(17) 0.0394(5) Uani 1 1 d .
H18 H -0.0487 0.7200 0.6675 0.047 Uiso 1 1 calc R
C16 C 0.1026(3) 0.9243(2) 0.85030(17) 0.0386(5) Uani 1 1 d .
H16 H 0.1657 1.0005 0.8658 0.046 Uiso 1 1 calc R
C10 C 0.1544(4) 0.4183(2) 0.66306(17) 0.0444(6) Uani 1 1 d .
H10 H 0.0907 0.3562 0.6879 0.053 Uiso 1 1 calc R
C4 C 0.5177(3) 0.7963(2) 0.72559(19) 0.0412(5) Uani 1 1 d .
C19 C -0.0853(3) 0.6987(2) 0.80696(17) 0.0382(5) Uani 1 1 d .
H19 H -0.1489 0.6226 0.7914 0.046 Uiso 1 1 calc R
C14 C -0.0525(3) 0.75202(19) 0.90445(16) 0.0332(5) Uani 1 1 d .
C20 C 0.1476(3) 0.9322(2) 0.67182(18) 0.0425(5) Uani 1 1 d .
H20A H 0.1359 0.8747 0.6118 0.051 Uiso 1 1 calc R
H20B H 0.2766 0.9577 0.6883 0.051 Uiso 1 1 calc R
C6 C 0.4521(4) 0.6985(3) 0.5570(2) 0.0543(7) Uani 1 1 d .
H6 H 0.4648 0.6983 0.4905 0.065 Uiso 1 1 calc R
C3 C 0.5959(3) 0.8910(2) 0.7982(2) 0.0489(6) Uani 1 1 d .
H3 H 0.6645 0.9567 0.7808 0.059 Uiso 1 1 calc R
C1 C 0.4642(3) 0.7877(2) 0.91992(19) 0.0412(5) Uani 1 1 d .
H1 H 0.4464 0.7860 0.9857 0.049 Uiso 1 1 calc R
C7 C 0.3458(3) 0.5995(2) 0.58716(17) 0.0425(5) Uani 1 1 d .
C2 C 0.5706(3) 0.8860(2) 0.8943(2) 0.0492(6) Uani 1 1 d .
H2 H 0.6239 0.9478 0.9429 0.059 Uiso 1 1 calc R
C9 C 0.1662(4) 0.4088(3) 0.56184(19) 0.0566(7) Uani 1 1 d .
H9 H 0.1106 0.3410 0.5203 0.068 Uiso 1 1 calc R
C8 C 0.2587(4) 0.4983(3) 0.52374(18) 0.0529(7) Uani 1 1 d .
H8 H 0.2642 0.4927 0.4563 0.064 Uiso 1 1 calc R
C5 C 0.5341(4) 0.7921(3) 0.6226(2) 0.0531(7) Uani 1 1 d .
H5 H 0.6022 0.8547 0.6005 0.064 Uiso 1 1 calc R
N1 N 0.3882(2) 0.69709(16) 0.85300(13) 0.0335(4) Uani 1 1 d .
N2 N 0.2317(2) 0.51368(16) 0.72463(13) 0.0337(4) Uani 1 1 d .
O5 O -0.1423(2) 1.01836(15) 0.59866(12) 0.0426(4) Uani 1 1 d .
O7 O 0.0592(2) 1.14923(14) 0.73823(12) 0.0460(4) Uani 1 1 d .
O6 O 0.1783(2) 1.11017(15) 0.57336(13) 0.0450(4) Uani 1 1 d .
O10 O 0.4014(4) 0.2061(2) 0.83778(19) 0.0720(6) Uani 1 1 d .
O8 O 0.4210(4) 0.8466(2) 0.34546(19) 0.0756(7) Uani 1 1 d .
O9 O 0.6837(5) 0.4100(3) 0.7058(2) 0.1189(11) Uani 1 1 d .
O3 O 0.1512(2) 0.77744(15) 1.12909(13) 0.0407(4) Uani 1 1 d .
H3A H 0.093(4) 0.801(2) 1.163(2) 0.037(8) Uiso 1 1 d .
H2B H 0.432(6) 0.375(4) 0.871(3) 0.098(15) Uiso 1 1 d .
H10B H 0.307(7) 0.202(4) 0.792(4) 0.125(18) Uiso 1 1 d .
H10A H 0.479(5) 0.187(3) 0.796(3) 0.083(12) Uiso 1 1 d .
H6A H 0.172(5) 1.072(3) 0.516(3) 0.093(13) Uiso 1 1 d .
H1A H 0.517(6) 0.452(4) 0.916(3) 0.069(17) Uiso 1 1 d .
H8A H 0.322(6) 0.881(4) 0.373(3) 0.106(14) Uiso 1 1 d .
H8B H 0.519(6) 0.866(4) 0.386(3) 0.104(15) 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'
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
O4 Cu1 O2 94.25(6) . .
O4 Cu1 N2 171.22(7) . .
O2 Cu1 N2 90.01(7) . .
O4 Cu1 N1 92.36(7) . .
O2 Cu1 N1 166.27(7) . .
N2 Cu1 N1 81.93(7) . .
O4 Cu1 O1 96.28(8) . .
O2 Cu1 O1 98.18(9) . .
N2 Cu1 O1 90.70(9) . .
N1 Cu1 O1 93.04(9) . .
O4 P1 O2 114.93(9) . 2_567
O4 P1 O3 105.95(10) . .
O2 P1 O3 108.79(9) 2_567 .
O4 P1 C13 110.05(10) . .
O2 P1 C13 109.03(10) 2_567 .
O3 P1 C13 107.83(11) . .
O7 P2 O5 115.48(10) . .
O7 P2 O6 107.29(10) . .
O5 P2 O6 110.64(10) . .
O7 P2 C20 110.03(11) . .
O5 P2 C20 110.08(11) . .
O6 P2 C20 102.51(11) . .
P1 O4 Cu1 133.60(9) . .
P1 O2 Cu1 137.82(10) 2_567 .
Cu1 O1 H2B 112(3) . .
Cu1 O1 H1A 136(5) . .
H2B O1 H1A 105(5) . .
N2 C11 C7 122.9(2) . .
N2 C11 C12 116.35(19) . .
C7 C11 C12 120.7(2) . .
C16 C15 C14 121.1(2) . .
C16 C15 H15 119.5 . .
C14 C15 H15 119.5 . .
C18 C17 C16 117.6(2) . .
C18 C17 C20 121.5(2) . .
C16 C17 C20 120.8(2) . .
C14 C13 P1 115.41(15) . .
C14 C13 H13A 108.4 . .
P1 C13 H13A 108.4 . .
C14 C13 H13B 108.4 . .
P1 C13 H13B 108.4 . .
H13A C13 H13B 107.5 . .
N1 C12 C4 123.2(2) . .
N1 C12 C11 116.62(19) . .
C4 C12 C11 120.1(2) . .
C17 C18 C19 121.4(2) . .
C17 C18 H18 119.3 . .
C19 C18 H18 119.3 . .
C15 C16 C17 121.2(2) . .
C15 C16 H16 119.4 . .
C17 C16 H16 119.4 . .
N2 C10 C9 121.6(2) . .
N2 C10 H10 119.2 . .
C9 C10 H10 119.2 . .
C12 C4 C3 117.0(2) . .
C12 C4 C5 118.6(2) . .
C3 C4 C5 124.5(2) . .
C18 C19 C14 120.9(2) . .
C18 C19 H19 119.6 . .
C14 C19 H19 119.6 . .
C19 C14 C15 117.9(2) . .
C19 C14 C13 121.0(2) . .
C15 C14 C13 121.1(2) . .
C17 C20 P2 116.89(16) . .
C17 C20 H20A 108.1 . .
P2 C20 H20A 108.1 . .
C17 C20 H20B 108.1 . .
P2 C20 H20B 108.1 . .
H20A C20 H20B 107.3 . .
C5 C6 C7 121.7(2) . .
C5 C6 H6 119.1 . .
C7 C6 H6 119.1 . .
C2 C3 C4 119.6(2) . .
C2 C3 H3 120.2 . .
C4 C3 H3 120.2 . .
N1 C1 C2 121.9(2) . .
N1 C1 H1 119.1 . .
C2 C1 H1 119.1 . .
C11 C7 C8 117.0(2) . .
C11 C7 C6 117.8(2) . .
C8 C7 C6 125.2(2) . .
C3 C2 C1 119.9(2) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C8 C9 C10 120.3(3) . .
C8 C9 H9 119.8 . .
C10 C9 H9 119.8 . .
C9 C8 C7 119.5(2) . .
C9 C8 H8 120.3 . .
C7 C8 H8 120.3 . .
C6 C5 C4 121.0(2) . .
C6 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
C1 N1 C12 118.4(2) . .
C1 N1 Cu1 129.32(17) . .
C12 N1 Cu1 112.20(15) . .
C10 N2 C11 118.62(19) . .
C10 N2 Cu1 128.59(15) . .
C11 N2 Cu1 112.79(15) . .
P2 O6 H6A 117(3) . .
H10B O10 H10A 95(4) . .
H8A O8 H8B 111(4) . .
P1 O3 H3A 111(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O4 1.9368(14) .
Cu1 O2 1.9406(15) .
Cu1 N2 2.0034(18) .
Cu1 N1 2.0202(18) .
Cu1 O1 2.285(2) .
P1 O4 1.5085(15) .
P1 O2 1.5097(15) 2_567
P1 O3 1.5660(17) .
P1 C13 1.804(2) .
P2 O7 1.5001(16) .
P2 O5 1.5056(18) .
P2 O6 1.5813(17) .
P2 C20 1.807(2) .
O2 P1 1.5097(15) 2_567
O1 H2B 0.84(5) .
O1 H1A 0.53(4) .
C11 N2 1.360(3) .
C11 C7 1.399(3) .
C11 C12 1.426(3) .
C15 C16 1.381(3) .
C15 C14 1.393(3) .
C15 H15 0.9300 .
C17 C18 1.387(3) .
C17 C16 1.392(3) .
C17 C20 1.512(3) .
C13 C14 1.508(3) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C12 N1 1.357(3) .
C12 C4 1.399(3) .
C18 C19 1.387(3) .
C18 H18 0.9300 .
C16 H16 0.9300 .
C10 N2 1.326(3) .
C10 C9 1.397(3) .
C10 H10 0.9300 .
C4 C3 1.405(4) .
C4 C5 1.431(4) .
C19 C14 1.387(3) .
C19 H19 0.9300 .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C6 C5 1.352(4) .
C6 C7 1.435(4) .
C6 H6 0.9300 .
C3 C2 1.363(4) .
C3 H3 0.9300 .
C1 N1 1.327(3) .
C1 C2 1.402(4) .
C1 H1 0.9300 .
C7 C8 1.406(4) .
C2 H2 0.9300 .
C9 C8 1.359(4) .
C9 H9 0.9300 .
C8 H8 0.9300 .
C5 H5 0.9300 .
O6 H6A 0.84(4) .
O10 H10B 0.92(5) .
O10 H10A 0.86(4) .
O8 H8A 0.95(5) .
O8 H8B 0.88(5) .
O3 H3A 0.70(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H10B O7 0.92(5) 1.93(5) 2.783(3) 153(4) 1_545
O10 H10A O8 0.86(4) 2.12(4) 2.928(3) 156(3) 2_666
O8 H8B O6 0.88(5) 2.26(5) 3.083(3) 154(4) 2_676
O8 H8A O5 0.95(5) 1.91(5) 2.825(3) 163(4) 2_576
O6 H6A O5 0.84(4) 1.74(4) 2.580(2) 173(4) 2_576
O3 H3A O7 0.70(3) 1.89(3) 2.580(2) 173(3) 2_577
