#------------------------------------------------------------------------------
#$Date: 2022-06-28 19:19:27 +0300 (Tue, 28 Jun 2022) $
#$Revision: 276344 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/83/4348314.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_4348314
loop_
_publ_author_name
'Rajakannu, Palanisamy'
'Howlader, Rana'
'Kalita, Alok Ch.'
'Butcher, Raymond J.'
'Murugavel, Ramaswamy'
_publ_section_title
;
 Role of 4,4′-bipyridine versus longer spacers
 4,4′-azobipyridine, 1,2-bis(4-pyridyl)ethylene, and
 1,2-bis(pyridin-3-ylmethylene)hydrazine in the formation of thermally
 labile metallophosphate coordination polymers
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              55
_journal_paper_doi               10.1039/C4QI00149D
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C28 H52 Co N4 O12 P2'
_chemical_formula_sum            'C28 H52 Co N4 O12 P2'
_chemical_formula_weight         757.61
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
;
2014-07-21 deposited with the CCDC.
2014-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                104.67(4)
_cell_angle_beta                 96.20(2)
_cell_angle_gamma                104.44(7)
_cell_formula_units_Z            1
_cell_length_a                   7.23(2)
_cell_length_b                   11.02(4)
_cell_length_c                   14.09(4)
_cell_measurement_reflns_used    2164
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.8
_cell_measurement_theta_min      2.8
_cell_volume                     1034(6)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       ω
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6894
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.8985
_exptl_absorpt_correction_T_min  0.8985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             401
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.189
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.366
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.366
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.1067
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3254
_refine_ls_wR_factor_ref         0.3401
_reflns_number_gt                3075
_reflns_number_total             3519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00149d2.cif
_cod_data_source_block           rk1-353
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1033(6)
_cod_database_code               4348314
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
Co1 Co 1.0000 0.0000 0.0000 0.0370(5) Uani 0.987(4) 2 d SP
P1 P 0.54123(18) 0.01835(12) 0.24462(9) 0.0414(5) Uani 1 1 d .
O1 O 0.7048(5) -0.0570(3) 0.2600(3) 0.0458(9) Uani 1 1 d .
O2 O 0.5812(6) 0.1386(4) 0.3437(3) 0.0549(10) Uani 1 1 d .
O3 O 0.5850(5) 0.0654(3) 0.1541(2) 0.0463(9) Uani 1 1 d .
O4 O 0.3386(5) -0.0675(4) 0.2383(3) 0.0525(10) Uani 1 1 d .
O5 O 0.9571(5) -0.0002(3) -0.1528(2) 0.0459(9) Uani 1 1 d .
O6 O 1.3083(5) 0.0737(3) 0.0081(2) 0.0418(8) Uani 1 1 d .
N1 N 0.9841(6) 0.2027(4) 0.0505(3) 0.0448(10) Uani 1 1 d .
N2 N 0.5935(6) 0.5001(4) 0.0244(3) 0.0482(11) Uani 1 1 d .
C1 C 0.8252(7) 0.2357(5) 0.0151(4) 0.0453(12) Uani 1 1 d .
H1 H 0.7248 0.1695 -0.0335 0.054 Uiso 1 1 calc R
C2 C 0.8022(7) 0.3622(4) 0.0467(4) 0.0411(11) Uani 1 1 d .
C3 C 0.9549(8) 0.4600(5) 0.1172(4) 0.0510(13) Uani 1 1 d .
H3 H 0.9476 0.5473 0.1399 0.061 Uiso 1 1 calc R
C4 C 1.1193(8) 0.4255(5) 0.1535(4) 0.0519(13) Uani 1 1 d .
H4 H 1.2224 0.4894 0.2021 0.062 Uiso 1 1 calc R
C5 C 1.1290(7) 0.2987(5) 0.1181(4) 0.0459(12) Uani 1 1 d .
H5 H 1.2416 0.2778 0.1420 0.055 Uiso 1 1 calc R
C6 C 0.6149(7) 0.3837(5) 0.0037(4) 0.0446(12) Uani 1 1 d .
C7 C 0.7093(7) -0.1462(5) 0.3262(4) 0.0458(12) Uani 1 1 d .
C8 C 0.6795(10) -0.0782(6) 0.4320(4) 0.0620(16) Uani 1 1 d .
H8A H 0.7817 0.0051 0.4605 0.093 Uiso 1 1 calc R
H8B H 0.6858 -0.1351 0.4749 0.093 Uiso 1 1 calc R
H8C H 0.5522 -0.0617 0.4273 0.093 Uiso 1 1 calc R
C9 C 0.5488(9) -0.2768(5) 0.2805(5) 0.0602(15) Uani 1 1 d .
H9A H 0.5679 -0.3191 0.2137 0.090 Uiso 1 1 calc R
H9B H 0.4216 -0.2602 0.2759 0.090 Uiso 1 1 calc R
H9C H 0.5547 -0.3343 0.3230 0.090 Uiso 1 1 calc R
C10 C 0.9135(9) -0.1684(7) 0.3284(6) 0.0716(19) Uani 1 1 d .
H10A H 1.0136 -0.0842 0.3572 0.107 Uiso 1 1 calc R
H10B H 0.9292 -0.2080 0.2602 0.107 Uiso 1 1 calc R
H10C H 0.9266 -0.2271 0.3690 0.107 Uiso 1 1 calc R
C11 C 0.7242(9) 0.2701(5) 0.3698(4) 0.0594(15) Uani 1 1 d .
C12 C 0.7316(11) 0.3288(7) 0.4828(5) 0.078(2) Uani 1 1 d .
H12A H 0.7770 0.2739 0.5195 0.118 Uiso 1 1 calc R
H12B H 0.6014 0.3318 0.4945 0.118 Uiso 1 1 calc R
H12C H 0.8211 0.4177 0.5058 0.118 Uiso 1 1 calc R
C13 C 0.6542(12) 0.3522(6) 0.3083(5) 0.076(2) Uani 1 1 d .
H13A H 0.6509 0.3119 0.2374 0.114 Uiso 1 1 calc R
H13B H 0.7434 0.4411 0.3296 0.114 Uiso 1 1 calc R
H13C H 0.5236 0.3558 0.3186 0.114 Uiso 1 1 calc R
C14 C 0.9309(9) 0.2557(7) 0.3526(6) 0.080(2) Uani 1 1 d .
H14A H 0.9699 0.2018 0.3921 0.120 Uiso 1 1 calc R
H14B H 1.0259 0.3426 0.3732 0.120 Uiso 1 1 calc R
H14C H 0.9252 0.2138 0.2817 0.120 Uiso 1 1 calc R
H5B H 1.0479 0.0318 -0.1818 0.080 Uiso 1 1 d .
H5A H 0.8692 -0.0641 -0.2197 0.080 Uiso 1 1 d .
H6A H 1.4024 0.1375 0.0770 0.080 Uiso 1 1 d .
H6B H 1.3550 0.0351 -0.0331 0.080 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'
Co Co 0.3494 0.9721 '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
O5 Co1 O5 180.00(19) . 2_755
O5 Co1 O6 91.11(14) . 2_755
O5 Co1 O6 88.89(14) 2_755 2_755
O5 Co1 O6 88.89(14) . .
O5 Co1 O6 91.11(14) 2_755 .
O6 Co1 O6 180.0 2_755 .
O5 Co1 N1 91.34(18) . .
O5 Co1 N1 88.66(18) 2_755 .
O6 Co1 N1 90.49(19) 2_755 .
O6 Co1 N1 89.51(19) . .
O5 Co1 N1 88.66(18) . 2_755
O5 Co1 N1 91.34(18) 2_755 2_755
O6 Co1 N1 89.51(19) 2_755 2_755
O6 Co1 N1 90.49(19) . 2_755
N1 Co1 N1 180.0(3) . 2_755
O4 P1 O3 117.6(2) . .
O4 P1 O2 105.8(2) . .
O3 P1 O2 111.7(3) . .
O4 P1 O1 111.7(3) . .
O3 P1 O1 103.0(2) . .
O2 P1 O1 106.7(3) . .
C7 O1 P1 126.8(3) . .
C11 O2 P1 128.5(4) . .
Co1 O5 H5B 124.2(3) . .
Co1 O5 H5A 135.8(3) . .
H5B O5 H5A 93.7(4) . .
Co1 O6 H6A 121.2(3) . .
Co1 O6 H6B 117.2(3) . .
H6A O6 H6B 118.3(4) . .
C5 N1 C1 117.7(5) . .
C5 N1 Co1 121.6(4) . .
C1 N1 Co1 120.7(3) . .
C6 N2 N2 111.7(5) . 2_665
N1 C1 C2 123.7(5) . .
N1 C1 H1 118.1 . .
C2 C1 H1 118.1 . .
C1 C2 C3 117.3(5) . .
C1 C2 C6 118.1(4) . .
C3 C2 C6 124.6(5) . .
C2 C3 C4 118.8(5) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
C5 C4 C3 119.8(5) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
N1 C5 C4 122.7(5) . .
N1 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
N2 C6 C2 120.2(5) . .
O1 C7 C9 110.1(5) . .
O1 C7 C8 109.7(5) . .
C9 C7 C8 109.8(5) . .
O1 C7 C10 104.7(4) . .
C9 C7 C10 110.7(6) . .
C8 C7 C10 111.7(5) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O2 C11 C13 109.7(5) . .
O2 C11 C12 104.2(5) . .
C13 C11 C12 111.8(6) . .
O2 C11 C14 109.9(5) . .
C13 C11 C14 111.8(6) . .
C12 C11 C14 109.1(6) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O5 2.141(8) .
Co1 O5 2.141(8) 2_755
Co1 O6 2.153(8) 2_755
Co1 O6 2.153(8) .
Co1 N1 2.201(8) .
Co1 N1 2.201(8) 2_755
P1 O4 1.512(6) .
P1 O3 1.528(5) .
P1 O2 1.604(5) .
P1 O1 1.631(5) .
O1 C7 1.520(7) .
O2 C11 1.485(7) .
O5 H5B 0.859(4) .
O5 H5A 1.048(4) .
O6 H6A 1.083(4) .
O6 H6B 0.788(4) .
N1 C5 1.358(7) .
N1 C1 1.370(8) .
N2 C6 1.293(8) .
N2 N2 1.449(9) 2_665
C1 C2 1.410(8) .
C1 H1 0.9500 .
C2 C3 1.412(8) .
C2 C6 1.520(8) .
C3 C4 1.419(9) .
C3 H3 0.9500 .
C4 C5 1.382(9) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C7 C9 1.538(8) .
C7 C8 1.554(9) .
C7 C10 1.554(9) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C13 1.534(10) .
C11 C12 1.548(10) .
C11 C14 1.579(10) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
O4 P1 O1 C7 -40.2(4) .
O3 P1 O1 C7 -167.3(4) .
O2 P1 O1 C7 74.9(4) .
O4 P1 O2 C11 -158.7(5) .
O3 P1 O2 C11 -29.6(5) .
O1 P1 O2 C11 82.2(5) .
O5 Co1 N1 C5 -124.6(4) .
O5 Co1 N1 C5 55.4(4) 2_755
O6 Co1 N1 C5 144.2(4) 2_755
O6 Co1 N1 C5 -35.8(4) .
N1 Co1 N1 C5 94(100) 2_755
O5 Co1 N1 C1 56.1(4) .
O5 Co1 N1 C1 -123.9(4) 2_755
O6 Co1 N1 C1 -35.0(4) 2_755
O6 Co1 N1 C1 145.0(4) .
N1 Co1 N1 C1 -85(100) 2_755
C5 N1 C1 C2 -1.5(7) .
Co1 N1 C1 C2 177.7(4) .
N1 C1 C2 C3 1.4(8) .
N1 C1 C2 C6 -177.9(4) .
C1 C2 C3 C4 -1.3(8) .
C6 C2 C3 C4 178.0(5) .
C2 C3 C4 C5 1.4(9) .
C1 N1 C5 C4 1.6(8) .
Co1 N1 C5 C4 -177.6(4) .
C3 C4 C5 N1 -1.6(9) .
N2 N2 C6 C2 179.4(5) 2_665
C1 C2 C6 N2 -174.6(5) .
C3 C2 C6 N2 6.1(8) .
P1 O1 C7 C9 71.6(6) .
P1 O1 C7 C8 -49.4(5) .
P1 O1 C7 C10 -169.4(4) .
P1 O2 C11 C13 74.1(7) .
P1 O2 C11 C12 -166.0(4) .
P1 O2 C11 C14 -49.3(7) .
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2022-06-28T19:18:00+03:00
;
 Removed the '_chemical_name_systematic' data item that had an incorrect value.
;
