#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:27:23 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232874 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/83/4348313.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_4348313
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         'C12 H18 N4 Ni O4, 2(C8 H18 O4 P)'
_chemical_formula_sum            'C28 H54 N4 Ni O12 P2'
_chemical_formula_weight         759.40
_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                104.485(5)
_cell_angle_beta                 96.215(8)
_cell_angle_gamma                103.909(3)
_cell_formula_units_Z            1
_cell_length_a                   7.026(3)
_cell_length_b                   10.737(5)
_cell_length_c                   13.782(6)
_cell_measurement_reflns_used    2163
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3
_cell_measurement_theta_min      2.2
_cell_volume                     961.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7304
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3351
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0372
_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)+(0.0839P)²+0.3105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                3259
_reflns_number_total             3351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00149d2.cif
_cod_data_source_block           rk1-370
_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.

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' 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_sg_symbol_H-M      P-1
_cod_database_code               4348313
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
Ni1 Ni 0.0000 0.0000 1.0000 0.01459(17) Uani 1 2 d S
P1 P 0.46001(9) -0.01773(6) 0.75570(4) 0.0194(2) Uani 1 1 d .
O1 O 0.2952(2) 0.05929(17) 0.74047(12) 0.0206(4) Uani 1 1 d .
O2 O 0.6636(3) 0.06879(19) 0.76181(14) 0.0275(4) Uani 1 1 d .
O4 O 0.4205(3) -0.13907(18) 0.65621(13) 0.0283(4) Uani 1 1 d .
O5 O 0.4171(2) -0.06589(17) 0.84661(12) 0.0223(4) Uani 1 1 d .
O6 O 0.0424(3) 0.00229(18) 1.15151(13) 0.0217(4) Uani 1 1 d .
O7 O 0.3019(2) 0.07379(17) 1.00672(13) 0.0187(4) Uani 1 1 d D
H7E H 0.3642 0.0676 1.0601 0.028 Uiso 1 1 calc RD
N1 N 0.0151(3) -0.19796(19) 0.95194(15) 0.0181(4) Uani 1 1 d .
N2 N 0.4057(3) -0.5010(2) 0.97530(17) 0.0268(5) Uani 1 1 d .
C1 C -0.1298(4) -0.2932(3) 0.8831(2) 0.0242(5) Uani 1 1 d .
H1 H -0.2436 -0.2702 0.8573 0.029 Uiso 1 1 calc R
C2 C -0.1208(4) -0.4240(3) 0.8478(2) 0.0289(6) Uani 1 1 d .
H2 H -0.2275 -0.4892 0.7994 0.035 Uiso 1 1 calc R
C3 C 0.0440(4) -0.4586(2) 0.8833(2) 0.0269(6) Uani 1 1 d .
H3 H 0.0529 -0.5478 0.8599 0.032 Uiso 1 1 calc R
C4 C 0.1969(4) -0.3606(2) 0.95408(18) 0.0209(5) Uani 1 1 d .
C5 C 0.1743(4) -0.2330(2) 0.98637(18) 0.0191(5) Uani 1 1 d .
H5 H 0.2777 -0.1664 1.0358 0.023 Uiso 1 1 calc R
C6 C 0.3816(4) -0.3835(3) 0.99607(19) 0.0243(5) Uani 1 1 d .
H6 H 0.4851 -0.3100 1.0394 0.029 Uiso 1 1 calc R
C7 C 0.0699(5) -0.2542(3) 0.6478(3) 0.0467(8) Uani 1 1 d .
H7A H 0.0729 -0.2200 0.7211 0.056 Uiso 1 1 calc R
H7B H -0.0297 -0.3415 0.6208 0.056 Uiso 1 1 calc R
H7C H 0.0352 -0.1913 0.6131 0.056 Uiso 1 1 calc R
C8 C 0.2754(5) -0.2697(3) 0.6299(2) 0.0347(7) Uani 1 1 d .
C9 C 0.2709(6) -0.3277(3) 0.5170(2) 0.0480(9) Uani 1 1 d .
H9A H 0.1834 -0.4195 0.4936 0.058 Uiso 1 1 calc R
H9B H 0.4060 -0.3283 0.5054 0.058 Uiso 1 1 calc R
H9C H 0.2206 -0.2728 0.4790 0.058 Uiso 1 1 calc R
C10 C 0.3451(6) -0.3537(3) 0.6917(3) 0.0524(9) Uani 1 1 d .
H10A H 0.2464 -0.4412 0.6747 0.063 Uiso 1 1 calc R
H10B H 0.3608 -0.3083 0.7644 0.063 Uiso 1 1 calc R
H10C H 0.4732 -0.3660 0.6759 0.063 Uiso 1 1 calc R
C11 C 0.2905(4) 0.1478(3) 0.67401(19) 0.0235(5) Uani 1 1 d .
C12 C 0.3176(5) 0.0793(3) 0.5681(2) 0.0390(7) Uani 1 1 d .
H12A H 0.2098 -0.0038 0.5389 0.047 Uiso 1 1 calc R
H12B H 0.4461 0.0585 0.5722 0.047 Uiso 1 1 calc R
H12C H 0.3144 0.1388 0.5248 0.047 Uiso 1 1 calc R
C13 C 0.0857(5) 0.1704(4) 0.6728(3) 0.0435(8) Uani 1 1 d .
H13A H 0.0755 0.2198 0.7413 0.052 Uiso 1 1 calc R
H13B H -0.0161 0.0838 0.6510 0.052 Uiso 1 1 calc R
H13C H 0.0652 0.2222 0.6252 0.052 Uiso 1 1 calc R
C14 C 0.4503(5) 0.2789(3) 0.7208(2) 0.0353(7) Uani 1 1 d .
H14A H 0.4238 0.3239 0.7870 0.042 Uiso 1 1 calc R
H14B H 0.4499 0.3363 0.6756 0.042 Uiso 1 1 calc R
H14C H 0.5807 0.2615 0.7300 0.042 Uiso 1 1 calc R
H6A H 0.124(6) -0.025(4) 1.177(3) 0.053(12) Uiso 1 1 d .
H6B H -0.057(6) -0.015(3) 1.176(3) 0.039(9) Uiso 1 1 d .
H7D H 0.334(4) 0.035(3) 0.9581(17) 0.026(8) Uiso 1 1 d 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'
Ni Ni 0.3393 1.1124 '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'
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
O7 Ni1 O7 180.0 2_557 .
O7 Ni1 O6 91.63(7) 2_557 2_557
O7 Ni1 O6 88.37(7) . 2_557
O7 Ni1 O6 88.37(7) 2_557 .
O7 Ni1 O6 91.63(7) . .
O6 Ni1 O6 180.000(1) 2_557 .
O7 Ni1 N1 91.66(7) 2_557 2_557
O7 Ni1 N1 88.34(7) . 2_557
O6 Ni1 N1 91.86(7) 2_557 2_557
O6 Ni1 N1 88.14(7) . 2_557
O7 Ni1 N1 88.34(7) 2_557 .
O7 Ni1 N1 91.66(7) . .
O6 Ni1 N1 88.14(7) 2_557 .
O6 Ni1 N1 91.86(7) . .
N1 Ni1 N1 180.000(1) 2_557 .
O2 P1 O5 117.50(10) . .
O2 P1 O4 106.08(11) . .
O5 P1 O4 111.34(11) . .
O2 P1 O1 111.09(11) . .
O5 P1 O1 103.50(9) . .
O4 P1 O1 106.95(10) . .
C11 O1 P1 126.60(15) . .
C8 O4 P1 128.50(17) . .
Ni1 O6 H6A 124(3) . .
Ni1 O6 H6B 117(3) . .
H6A O6 H6B 109(4) . .
Ni1 O7 H7E 109.5 . .
Ni1 O7 H7D 110(2) . .
H7E O7 H7D 111.3 . .
C1 N1 C5 117.3(2) . .
C1 N1 Ni1 121.50(16) . .
C5 N1 Ni1 121.12(16) . .
C6 N2 N2 111.0(3) . 2_647
N1 C1 C2 122.7(2) . .
N1 C1 H1 118.7 . .
C2 C1 H1 118.7 . .
C3 C2 C1 119.5(2) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
C2 C3 C4 118.6(2) . .
C2 C3 H3 120.7 . .
C4 C3 H3 120.7 . .
C5 C4 C3 118.1(2) . .
C5 C4 C6 117.9(2) . .
C3 C4 C6 124.1(2) . .
N1 C5 C4 123.8(2) . .
N1 C5 H5 118.1 . .
C4 C5 H5 118.1 . .
N2 C6 C4 121.0(2) . .
N2 C6 H6 119.5 . .
C4 C6 H6 119.5 . .
C8 C7 H7A 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C8 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
O4 C8 C10 109.4(3) . .
O4 C8 C9 103.9(2) . .
C10 C8 C9 111.6(3) . .
O4 C8 C7 110.4(2) . .
C10 C8 C7 111.2(3) . .
C9 C8 C7 110.0(3) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O1 C11 C14 109.5(2) . .
O1 C11 C13 104.0(2) . .
C14 C11 C13 110.3(3) . .
O1 C11 C12 110.2(2) . .
C14 C11 C12 111.3(2) . .
C13 C11 C12 111.3(2) . .
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
Ni1 O7 2.0609(18) 2_557
Ni1 O7 2.0609(18) .
Ni1 O6 2.070(2) 2_557
Ni1 O6 2.070(2) .
Ni1 N1 2.095(2) 2_557
Ni1 N1 2.095(2) .
P1 O2 1.487(2) .
P1 O5 1.5030(19) .
P1 O4 1.5825(19) .
P1 O1 1.6009(17) .
O1 C11 1.479(3) .
O4 C8 1.454(3) .
O6 H6A 0.79(4) .
O6 H6B 0.81(4) .
O7 H7E 0.8400 .
O7 H7D 0.783(18) .
N1 C1 1.337(3) .
N1 C5 1.340(3) .
N2 C6 1.278(3) .
N2 N2 1.416(4) 2_647
C1 C2 1.386(4) .
C1 H1 0.9500 .
C2 C3 1.376(4) .
C2 H2 0.9500 .
C3 C4 1.390(4) .
C3 H3 0.9500 .
C4 C5 1.384(3) .
C4 C6 1.463(3) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.531(5) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C10 1.511(5) .
C8 C9 1.519(4) .
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 C14 1.512(4) .
C11 C13 1.515(4) .
C11 C12 1.516(4) .
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_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
C10 H10B O5 0.98 2.48 3.175(4) 127.7
C14 H14C O2 0.98 2.41 3.120(4) 129.3
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
O2 P1 O1 C11 40.9(2) .
O5 P1 O1 C11 167.88(18) .
O4 P1 O1 C11 -74.4(2) .
O2 P1 O4 C8 160.1(2) .
O5 P1 O4 C8 31.1(3) .
O1 P1 O4 C8 -81.3(2) .
O7 Ni1 N1 C1 37.60(19) 2_557
O7 Ni1 N1 C1 -142.40(19) .
O6 Ni1 N1 C1 -54.09(19) 2_557
O6 Ni1 N1 C1 125.91(19) .
N1 Ni1 N1 C1 -156(100) 2_557
O7 Ni1 N1 C5 -144.89(18) 2_557
O7 Ni1 N1 C5 35.11(18) .
O6 Ni1 N1 C5 123.42(19) 2_557
O6 Ni1 N1 C5 -56.58(19) .
N1 Ni1 N1 C5 22(100) 2_557
C5 N1 C1 C2 0.4(4) .
Ni1 N1 C1 C2 178.0(2) .
N1 C1 C2 C3 -0.8(4) .
C1 C2 C3 C4 0.1(4) .
C2 C3 C4 C5 0.9(4) .
C2 C3 C4 C6 -178.6(2) .
C1 N1 C5 C4 0.6(4) .
Ni1 N1 C5 C4 -177.00(18) .
C3 C4 C5 N1 -1.3(4) .
C6 C4 C5 N1 178.2(2) .
N2 N2 C6 C4 -179.6(2) 2_647
C5 C4 C6 N2 174.8(2) .
C3 C4 C6 N2 -5.8(4) .
P1 O4 C8 C10 -74.8(3) .
P1 O4 C8 C9 165.9(2) .
P1 O4 C8 C7 48.0(3) .
P1 O1 C11 C14 -72.9(3) .
P1 O1 C11 C13 169.2(2) .
P1 O1 C11 C12 49.8(3) .
