#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:56:56 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179605 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/69/4506941.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_4506941
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         'C18 H20 Cu N2 O7 P2'
_chemical_formula_sum            'C18 H20 Cu N2 O7 P2'
_chemical_formula_weight         501.84
_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                110.125(2)
_cell_angle_beta                 108.317(2)
_cell_angle_gamma                92.168(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9763(11)
_cell_length_b                   10.1710(11)
_cell_length_c                   11.3001(13)
_cell_measurement_reflns_used    5888
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.18
_cell_volume                     1008.3(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10437
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.8609
_exptl_absorpt_correction_T_min  0.7146
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0342
_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)+(0.0563P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                3276
_reflns_number_total             3908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3011162_si_002.cif
_cod_data_source_block           compound-4
_cod_original_cell_volume        1008.26(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4506941
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 0.75362(3) 0.86709(3) 0.95458(3) 0.02629(11) Uani 1 1 d .
O4 O 0.83296(18) 1.01059(18) 0.90616(16) 0.0279(4) Uani 1 1 d .
N1 N 0.5538(2) 0.8795(2) 0.8515(2) 0.0284(5) Uani 1 1 d .
O1 O 0.78847(19) 0.68528(19) 0.78640(18) 0.0340(4) Uani 1 1 d .
N2 N 0.6438(2) 0.7649(2) 1.0272(2) 0.0319(5) Uani 1 1 d .
C6 C 0.5010(3) 0.7641(3) 0.9852(3) 0.0324(6) Uani 1 1 d .
C5 C 0.4496(3) 0.8285(3) 0.8848(2) 0.0290(6) Uani 1 1 d .
P2 P 0.93491(6) 1.00740(7) 0.83114(6) 0.02465(16) Uani 1 1 d .
P1 P 0.68310(7) 0.58030(7) 0.65525(7) 0.03011(17) Uani 1 1 d .
O3 O 0.98214(18) 0.85907(19) 0.78716(17) 0.0317(4) Uani 1 1 d .
H30 H 0.9115 0.7983 0.7376 0.048 Uiso 1 1 calc R
O2 O 0.93324(18) 0.87964(19) 1.09524(17) 0.0308(4) Uani 1 1 d .
O5 O 0.5528(2) 0.5163(2) 0.67281(19) 0.0395(5) Uani 1 1 d .
O6 O 0.6401(2) 0.6513(2) 0.55159(19) 0.0396(5) Uani 1 1 d .
H6 H 0.5830 0.5943 0.4805 0.059 Uiso 1 1 calc R
C18 C 1.0021(3) 0.8677(3) 0.4135(3) 0.0328(6) Uani 1 1 d .
H18 H 1.0036 0.7775 0.3554 0.039 Uiso 1 1 calc R
C16 C 0.9196(3) 1.0150(3) 0.5838(2) 0.0301(6) Uani 1 1 d .
C10 C 0.7005(3) 0.7089(3) 1.1189(3) 0.0437(7) Uani 1 1 d .
H10 H 0.7986 0.7084 1.1473 0.052 Uiso 1 1 calc R
C1 C 0.5169(3) 0.9378(3) 0.7593(3) 0.0376(7) Uani 1 1 d .
H1 H 0.5886 0.9739 0.7371 0.045 Uiso 1 1 calc R
C15 C 0.8367(3) 1.0308(3) 0.6782(2) 0.0340(6) Uani 1 1 d .
H15A H 0.7494 0.9616 0.6318 0.041 Uiso 1 1 calc R
H15B H 0.8096 1.1244 0.7008 0.041 Uiso 1 1 calc R
C4 C 0.3084(3) 0.8393(3) 0.8273(3) 0.0383(7) Uani 1 1 d .
H4 H 0.2383 0.8068 0.8534 0.046 Uiso 1 1 calc R
C3 C 0.2722(3) 0.8983(3) 0.7313(3) 0.0425(7) Uani 1 1 d .
H3 H 0.1774 0.9053 0.6910 0.051 Uiso 1 1 calc R
C2 C 0.3780(3) 0.9468(3) 0.6956(3) 0.0435(7) Uani 1 1 d .
H2 H 0.3556 0.9851 0.6294 0.052 Uiso 1 1 calc R
C11 C 0.7717(3) 0.4353(3) 0.5909(3) 0.0451(8) Uani 1 1 d .
H11A H 0.8106 0.3975 0.6603 0.054 Uiso 1 1 calc R
H11B H 0.7004 0.3607 0.5154 0.054 Uiso 1 1 calc R
C17 C 0.9219(3) 0.8830(3) 0.4962(3) 0.0336(6) Uani 1 1 d .
H17 H 0.8692 0.8033 0.4923 0.040 Uiso 1 1 calc R
C12 C 0.8907(3) 0.4700(3) 0.5454(3) 0.0396(7) Uani 1 1 d .
C14 C 0.8597(3) 0.4688(3) 0.4163(3) 0.0428(7) Uani 1 1 d .
H14 H 0.7651 0.4480 0.3586 0.051 Uiso 1 1 calc R
C13 C 1.0318(3) 0.5018(3) 0.6277(3) 0.0423(7) Uani 1 1 d .
H13 H 1.0551 0.5037 0.7147 0.051 Uiso 1 1 calc R
C7 C 0.4139(3) 0.7066(3) 1.0356(3) 0.0492(8) Uani 1 1 d .
H7 H 0.3157 0.7058 1.0052 0.059 Uiso 1 1 calc R
C8 C 0.4745(4) 0.6508(4) 1.1310(4) 0.0560(9) Uani 1 1 d .
H8 H 0.4178 0.6128 1.1667 0.067 Uiso 1 1 calc R
C9 C 0.6187(4) 0.6517(4) 1.1729(3) 0.0552(9) Uani 1 1 d .
H9 H 0.6613 0.6140 1.2372 0.066 Uiso 1 1 calc R
O7 O 0.0480(5) 0.6158(5) -0.0341(5) 0.1233(13) Uani 1 1 d .
H7A H 0.094(3) 0.636(3) 0.059(3) 0.028(8) 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 93.46(7) . .
O4 Cu1 N1 91.38(8) . .
O2 Cu1 N1 164.99(8) . .
O4 Cu1 N2 163.45(8) . .
O2 Cu1 N2 91.43(8) . .
N1 Cu1 N2 80.19(9) . .
O4 Cu1 O1 92.70(7) . .
O2 Cu1 O1 96.69(7) . .
N1 Cu1 O1 97.26(8) . .
N2 Cu1 O1 102.42(8) . .
P2 O4 Cu1 132.12(11) . .
C1 N1 C5 118.5(2) . .
C1 N1 Cu1 125.95(18) . .
C5 N1 Cu1 115.49(17) . .
P1 O1 Cu1 130.92(10) . .
C10 N2 C6 118.7(2) . .
C10 N2 Cu1 125.75(19) . .
C6 N2 Cu1 115.35(18) . .
N2 C6 C7 121.2(3) . .
N2 C6 C5 114.4(2) . .
C7 C6 C5 124.4(3) . .
N1 C5 C4 121.1(3) . .
N1 C5 C6 114.3(2) . .
C4 C5 C6 124.6(2) . .
O4 P2 O2 115.49(10) . 2_777
O4 P2 O3 111.09(10) . .
O2 P2 O3 108.88(10) 2_777 .
O4 P2 C15 106.94(11) . .
O2 P2 C15 107.93(12) 2_777 .
O3 P2 C15 106.03(12) . .
O1 P1 O5 112.63(11) . .
O1 P1 O6 109.55(11) . .
O5 P1 O6 112.03(12) . .
O1 P1 C11 108.23(14) . .
O5 P1 C11 106.84(13) . .
O6 P1 C11 107.33(13) . .
P2 O2 Cu1 131.46(11) 2_777 .
C17 C18 C16 120.9(3) . 2_776
C17 C16 C18 118.6(2) . 2_776
C17 C16 C15 120.4(2) . .
C18 C16 C15 121.0(3) 2_776 .
N2 C10 C9 122.2(3) . .
N1 C1 C2 122.9(3) . .
C16 C15 P2 113.66(17) . .
C3 C4 C5 119.5(3) . .
C2 C3 C4 119.1(3) . .
C1 C2 C3 118.8(3) . .
C12 C11 P1 116.2(2) . .
C16 C17 C18 120.5(3) . .
C13 C12 C14 117.8(3) . .
C13 C12 C11 122.0(3) . .
C14 C12 C11 120.2(3) . .
C13 C14 C12 120.8(3) 2_766 .
C12 C13 C14 121.4(3) . 2_766
C8 C7 C6 119.2(3) . .
C9 C8 C7 119.3(3) . .
C8 C9 C10 119.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O4 1.9470(17) .
Cu1 O2 1.9511(17) .
Cu1 N1 2.001(2) .
Cu1 N2 2.005(2) .
Cu1 O1 2.2799(18) .
O4 P2 1.5099(17) .
N1 C1 1.332(3) .
N1 C5 1.353(3) .
O1 P1 1.5127(18) .
N2 C10 1.334(4) .
N2 C6 1.352(3) .
C6 C7 1.386(4) .
C6 C5 1.467(4) .
C5 C4 1.379(4) .
P2 O2 1.5108(18) 2_777
P2 O3 1.5588(19) .
P2 C15 1.800(3) .
P1 O5 1.5299(18) .
P1 O6 1.538(2) .
P1 C11 1.802(3) .
O2 P2 1.5107(17) 2_777
C18 C17 1.384(4) .
C18 C16 1.388(4) 2_776
C16 C17 1.373(4) .
C16 C18 1.388(4) 2_776
C16 C15 1.514(3) .
C10 C9 1.379(4) .
C1 C2 1.369(4) .
C4 C3 1.374(4) .
C3 C2 1.372(4) .
C11 C12 1.508(4) .
C12 C13 1.374(4) .
C12 C14 1.389(4) .
C14 C13 1.387(4) 2_766
C13 C14 1.387(4) 2_766
C7 C8 1.373(5) .
C8 C9 1.364(5) .
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
O6 H6 O5 0.82 1.78 2.598(3) 174.2 2_666
