#------------------------------------------------------------------------------
#$Date: 2016-02-05 00:41:09 +0200 (Fri, 05 Feb 2016) $
#$Revision: 175978 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/33/7223332.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_7223332
loop_
_publ_author_name
'Narang, Shikha'
'Singh, Udai P.'
'Venugopalan, P.'
_publ_section_title
;
 Solvent-mediated supramolecular templated assembly of a metal
 organophosphonate via a crystal--amorphous--crystal transformation
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              54
_journal_paper_doi               10.1039/C5CE01594D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C54 H52 Cu2 N4 O8 P2, 2(N O3), 4(C H4 O)'
_chemical_formula_sum            'C58 H68 Cu2 N6 O18 P2'
_chemical_formula_weight         1324.3
_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
_audit_update_record
;
2015-11-06 deposited with the CCDC.
2015-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                117.067(4)
_cell_angle_beta                 101.070(4)
_cell_angle_gamma                101.147(4)
_cell_formula_units_Z            1
_cell_length_a                   11.3974(12)
_cell_length_b                   11.5337(12)
_cell_length_c                   12.5848(13)
_cell_measurement_reflns_used    103
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.34
_cell_volume                     1369.1(3)
_computing_cell_refinement       'Bruker kappa Apex'
_computing_data_collection       'Bruker kappa Apex'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker XSHELL'
_computing_publication_material  'Bruker XSHELL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16802
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.61
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.531
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0516P)²+6.7610P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1610
_reflns_number_gt                4340
_reflns_number_total             5127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01594d3.cif
_cod_data_source_block           1dash
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7223327--7223332.cif.
;
_cod_original_cell_volume        1369.1(2)
_cod_database_code               7223332
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 0.48170(5) 0.99088(6) 0.19451(5) 0.01178(18) Uani 1 1 d . . 4
P1 P 0.33466(11) 0.85125(12) -0.10875(11) 0.0119(3) Uani 1 1 d . A 4
O1 O 0.4259(3) 0.8826(3) 0.0114(3) 0.0151(7) Uani 1 1 d . A 4
O2 O 0.2430(3) 0.6968(3) -0.1768(3) 0.0154(7) Uani 1 1 d . A 4
O3 O 0.3917(3) 0.8627(3) -0.2034(3) 0.0142(7) Uani 1 1 d . . 4
O4 O 0.6175(3) 0.8782(4) 0.2093(4) 0.0293(9) Uani 1 1 d . B 4
O5 O 0.8514(7) 1.0153(8) 0.3880(7) 0.0317(18) Uiso 0.50 1 d PDU C -1
O5A O 0.851(2) 0.9214(16) 0.420(2) 0.173(7) Uiso 0.50 1 d PDU D -2
O6 O 1.0368(8) 1.0787(9) 0.5265(9) 0.047(2) Uiso 0.50 1 d PDU C -1
O6A O 0.8492(8) 1.0880(9) 0.3848(8) 0.040(2) Uiso 0.50 1 d PDU D -2
O7 O 0.9099(10) 0.8716(9) 0.4369(11) 0.065(3) Uiso 0.50 1 d PDU C -1
O7A O 0.9925(18) 1.121(2) 0.5475(17) 0.156(6) Uiso 0.50 1 d PDU D -2
N1 N 0.3422(4) 0.8690(4) 0.2098(4) 0.0160(8) Uani 1 1 d . E 4
N2 N 0.4984(4) 1.1115(4) 0.3765(4) 0.0140(8) Uani 1 1 d . E 4
N3 N 0.9341(7) 0.9901(8) 0.4534(8) 0.028(2) Uiso 0.50 1 d PDU C -1
N3A N 0.8931(16) 1.0464(16) 0.4540(15) 0.131(6) Uiso 0.50 1 d PDU D -2
C1 C 0.2262(4) 0.9486(5) -0.0834(4) 0.0143(9) Uani 1 1 d . A 4
H1A H 0.2672 1.0366 -0.0733 0.017 Uiso 1 1 calc R A 4
H1B H 0.1538 0.9007 -0.1593 0.017 Uiso 1 1 calc R A 4
C2 C 0.1777(4) 0.9763(5) 0.0272(5) 0.0153(10) Uani 1 1 d . A 4
C3 C 0.0713(4) 0.8777(5) 0.0136(5) 0.0153(10) Uani 1 1 d . A 4
C4 C 0.0052(4) 0.7503(5) -0.1021(5) 0.0178(10) Uani 1 1 d . A 4
H4 H 0.0336 0.7290 -0.1711 0.021 Uiso 1 1 calc R A 4
C5 C -0.0987(5) 0.6600(5) -0.1118(5) 0.0222(11) Uani 1 1 d . A 4
H5 H -0.1396 0.5774 -0.1875 0.027 Uiso 1 1 calc R A 4
C6 C -0.1462(5) 0.6890(5) -0.0089(5) 0.0220(11) Uani 1 1 d . A 4
H6 H -0.2190 0.6271 -0.0187 0.026 Uiso 1 1 calc R A 4
C7 C -0.0856(5) 0.8064(5) 0.1027(5) 0.0226(11) Uani 1 1 d . A 4
H7 H -0.1153 0.8235 0.1705 0.027 Uiso 1 1 calc R A 4
C8 C 0.0244(4) 0.9051(5) 0.1180(5) 0.0164(10) Uani 1 1 d . A 4
C9 C 0.0851(5) 1.0279(5) 0.2332(5) 0.0179(10) Uani 1 1 d . A 4
H9 H 0.0553 1.0444 0.3008 0.021 Uiso 1 1 calc R A 4
C10 C 0.1895(5) 1.1257(5) 0.2478(5) 0.0158(10) Uani 1 1 d . A 4
C11 C 0.2495(5) 1.2510(5) 0.3655(5) 0.0192(10) Uani 1 1 d . A 4
H11 H 0.2210 1.2647 0.4335 0.023 Uiso 1 1 calc R A 4
C12 C 0.3475(5) 1.3505(5) 0.3797(5) 0.0214(11) Uani 1 1 d . A 4
H12 H 0.3848 1.4327 0.4564 0.026 Uiso 1 1 calc R A 4
C13 C 0.3930(5) 1.3287(5) 0.2775(5) 0.0207(11) Uani 1 1 d . A 4
H13 H 0.4597 1.3980 0.2881 0.025 Uiso 1 1 calc R A 4
C14 C 0.3418(4) 1.2090(5) 0.1638(5) 0.0167(10) Uani 1 1 d . A 4
H14 H 0.3750 1.1975 0.0990 0.020 Uiso 1 1 calc R A 4
C15 C 0.2375(4) 1.1010(5) 0.1434(5) 0.0147(10) Uani 1 1 d . A 4
C16 C 0.2988(5) 0.5871(5) -0.2156(5) 0.0238(11) Uani 1 1 d . A 4
H16A H 0.3759 0.6125 -0.1500 0.029 Uiso 1 1 calc R A 4
H16B H 0.3192 0.5703 -0.2916 0.029 Uiso 1 1 calc R A 4
C17 C 0.2040(6) 0.4592(5) -0.2397(6) 0.0328(14) Uani 1 1 d . A 4
H17A H 0.1890 0.4746 -0.1625 0.049 Uiso 1 1 calc R A 4
H17B H 0.2365 0.3836 -0.2710 0.049 Uiso 1 1 calc R A 4
H17C H 0.1263 0.4382 -0.3008 0.049 Uiso 1 1 calc R A 4
C18 C 0.2692(5) 0.7418(5) 0.1181(5) 0.0186(10) Uani 1 1 d . E 4
H18 H 0.2848 0.7031 0.0415 0.022 Uiso 1 1 calc R E 4
C19 C 0.1715(5) 0.6666(5) 0.1341(5) 0.0228(11) Uani 1 1 d . E 4
H19 H 0.1206 0.5795 0.0683 0.027 Uiso 1 1 calc R E 4
C20 C 0.1502(5) 0.7221(6) 0.2490(6) 0.0250(12) Uani 1 1 d . E 4
H20 H 0.0859 0.6720 0.2620 0.030 Uiso 1 1 calc R E 4
C21 C 0.2260(5) 0.8535(6) 0.3446(5) 0.0222(11) Uani 1 1 d . E 4
H21 H 0.2123 0.8935 0.4220 0.027 Uiso 1 1 calc R E 4
C22 C 0.3230(5) 0.9246(5) 0.3229(5) 0.0165(10) Uani 1 1 d . E 4
C23 C 0.4113(5) 1.0616(5) 0.4165(5) 0.0176(10) Uani 1 1 d . E 4
C24 C 0.4083(5) 1.1370(6) 0.5394(5) 0.0225(11) Uani 1 1 d . E 4
H24 H 0.3465 1.1019 0.5654 0.027 Uiso 1 1 calc R E 4
C25 C 0.4986(5) 1.2642(6) 0.6217(5) 0.0246(11) Uani 1 1 d . E 4
H25 H 0.4991 1.3158 0.7041 0.030 Uiso 1 1 calc R E 4
C26 C 0.5880(5) 1.3135(5) 0.5792(5) 0.0220(11) Uani 1 1 d . E 4
H26 H 0.6497 1.3989 0.6330 0.026 Uiso 1 1 calc R E 4
C27 C 0.5852(5) 1.2351(5) 0.4561(5) 0.0177(10) Uani 1 1 d . E 4
H27 H 0.6452 1.2692 0.4279 0.021 Uiso 1 1 calc R E 4
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
O3 Cu1 O1 93.70(14) 2_675 .
O3 Cu1 N1 168.97(15) 2_675 .
O1 Cu1 N1 94.05(15) . .
O3 Cu1 N2 90.58(15) 2_675 .
O1 Cu1 N2 165.82(15) . .
N1 Cu1 N2 80.08(16) . .
O3 Cu1 O4 93.21(14) 2_675 .
O1 Cu1 O4 91.65(15) . .
N1 Cu1 O4 94.39(15) . .
N2 Cu1 O4 101.61(16) . .
O1 P1 O3 116.18(19) . .
O1 P1 O2 108.32(19) . .
O3 P1 O2 106.70(18) . .
O1 P1 C1 113.2(2) . .
O3 P1 C1 108.8(2) . .
O2 P1 C1 102.5(2) . .
P1 O1 Cu1 146.0(2) . .
C16 O2 P1 118.0(3) . .
P1 O3 Cu1 133.3(2) . 2_675
C18 N1 C22 119.6(4) . .
C18 N1 Cu1 125.2(3) . .
C22 N1 Cu1 115.1(3) . .
C27 N2 C23 119.5(4) . .
C27 N2 Cu1 125.3(3) . .
C23 N2 Cu1 115.2(3) . .
O6 N3 O7 120.5(8) . .
O6 N3 O5 121.2(8) . .
O7 N3 O5 118.2(8) . .
O6A N3A O5A 119.7(10) . .
O6A N3A O7A 121.0(10) . .
O5A N3A O7A 118.4(10) . .
C2 C1 P1 118.1(3) . .
C15 C2 C3 119.8(4) . .
C15 C2 C1 120.2(4) . .
C3 C2 C1 120.0(4) . .
C2 C3 C4 122.6(5) . .
C2 C3 C8 119.9(4) . .
C4 C3 C8 117.5(4) . .
C5 C4 C3 120.6(5) . .
C4 C5 C6 121.6(5) . .
C7 C6 C5 119.9(5) . .
C6 C7 C8 120.7(5) . .
C9 C8 C7 120.4(5) . .
C9 C8 C3 120.0(4) . .
C7 C8 C3 119.6(5) . .
C10 C9 C8 120.8(5) . .
C9 C10 C11 120.0(5) . .
C9 C10 C15 120.2(4) . .
C11 C10 C15 119.7(5) . .
C12 C11 C10 120.9(5) . .
C11 C12 C13 119.7(5) . .
C14 C13 C12 122.0(5) . .
C13 C14 C15 120.5(5) . .
C2 C15 C14 123.5(5) . .
C2 C15 C10 119.4(4) . .
C14 C15 C10 117.1(4) . .
O2 C16 C17 108.0(4) . .
N1 C18 C19 121.8(5) . .
C18 C19 C20 119.3(5) . .
C19 C20 C21 119.0(5) . .
C20 C21 C22 119.1(5) . .
N1 C22 C21 121.1(5) . .
N1 C22 C23 114.5(4) . .
C21 C22 C23 124.4(5) . .
N2 C23 C24 121.4(5) . .
N2 C23 C22 114.9(4) . .
C24 C23 C22 123.7(5) . .
C25 C24 C23 119.0(5) . .
C24 C25 C26 118.8(5) . .
C25 C26 C27 119.6(5) . .
N2 C27 C26 121.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O3 1.942(3) 2_675
Cu1 O1 1.945(3) .
Cu1 N1 2.011(4) .
Cu1 N2 2.012(4) .
Cu1 O4 2.237(4) .
P1 O1 1.501(3) .
P1 O3 1.506(3) .
P1 O2 1.595(3) .
P1 C1 1.803(5) .
O2 C16 1.454(6) .
O3 Cu1 1.942(3) 2_675
O5 N3 1.295(8) .
O5A N3A 1.260(9) .
O6 N3 1.236(8) .
O6A N3A 1.243(9) .
O7 N3 1.250(8) .
O7A N3A 1.264(9) .
N1 C18 1.339(6) .
N1 C22 1.352(6) .
N2 C27 1.337(6) .
N2 C23 1.343(6) .
C1 C2 1.518(7) .
C2 C15 1.413(7) .
C2 C3 1.416(7) .
C3 C4 1.432(7) .
C3 C8 1.438(7) .
C4 C5 1.361(7) .
C5 C6 1.424(8) .
C6 C7 1.349(8) .
C7 C8 1.436(7) .
C8 C9 1.398(7) .
C9 C10 1.388(7) .
C10 C11 1.426(7) .
C10 C15 1.450(7) .
C11 C12 1.356(8) .
C12 C13 1.413(8) .
C13 C14 1.366(7) .
C14 C15 1.432(7) .
C16 C17 1.512(7) .
C18 C19 1.380(7) .
C19 C20 1.383(8) .
C20 C21 1.388(8) .
C21 C22 1.392(7) .
C22 C23 1.460(7) .
C23 C24 1.400(7) .
C24 C25 1.381(8) .
C25 C26 1.382(8) .
C26 C27 1.383(7) .
