#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:28:27 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232876 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/83/4348325.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_4348325
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         'C36 H56 Mn N8 O10 P2'
_chemical_formula_sum            'C36 H56 Mn N8 O10 P2'
_chemical_formula_weight         877.77
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-06-04 deposited with the CCDC.
2014-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.043(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.7719(17)
_cell_length_b                   13.6473(6)
_cell_length_c                   11.1274(7)
_cell_measurement_reflns_used    7948
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7797
_cell_measurement_theta_min      3.3038
_cell_volume                     4273.7(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14839
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         1.795
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3753
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0474
_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)+(0.0973P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                2830
_reflns_number_total             3753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00149d3.cif
_cod_data_source_block           1_shelxl
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4348325
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Mn1 Mn 0.7500 0.7500 0.5000 0.01874(18) Uani 1 2 d S
P1 P 0.85783(2) 0.76348(5) 0.70529(7) 0.0235(2) Uani 1 1 d .
O1 O 0.82391(6) 0.72663(13) 0.58220(18) 0.0272(4) Uani 1 1 d .
O2 O 0.83818(7) 0.78066(14) 0.80992(19) 0.0317(5) Uani 1 1 d .
O3 O 0.88048(6) 0.85879(13) 0.66655(18) 0.0291(5) Uani 1 1 d .
O4 O 0.90337(6) 0.69498(13) 0.75003(19) 0.0301(5) Uani 1 1 d .
O5 O 0.75775(6) 0.75036(12) 0.31109(19) 0.0277(4) Uani 1 1 d D
N1 N 0.74204(7) 0.58132(15) 0.4895(2) 0.0238(5) Uani 1 1 d .
N2 N 0.74142(8) 0.27435(16) 0.5338(2) 0.0247(5) Uani 1 1 d .
N3 N 0.84717(8) 0.73707(16) 0.2468(3) 0.0325(6) Uani 1 1 d .
N4 N 0.99458(8) 0.73573(17) 0.2988(2) 0.0334(6) Uani 1 1 d .
C1 C 0.90910(9) 0.9344(2) 0.7488(3) 0.0303(7) Uani 1 1 d .
C2 C 0.93077(12) 0.9899(2) 0.6635(3) 0.0442(8) Uani 1 1 d .
H2A H 0.9059 1.0171 0.5930 0.066 Uiso 1 1 calc R
H2B H 0.9497 0.9460 0.6326 0.066 Uiso 1 1 calc R
H2C H 0.9504 1.0418 0.7109 0.066 Uiso 1 1 calc R
C3 C 0.87642(12) 1.0010(2) 0.7913(4) 0.0461(8) Uani 1 1 d .
H3A H 0.8628 0.9651 0.8452 0.069 Uiso 1 1 calc R
H3B H 0.8515 1.0245 0.7182 0.069 Uiso 1 1 calc R
H3C H 0.8942 1.0556 0.8374 0.069 Uiso 1 1 calc R
C4 C 0.94722(11) 0.8904(2) 0.8621(3) 0.0438(8) Uani 1 1 d .
H4A H 0.9325 0.8554 0.9141 0.066 Uiso 1 1 calc R
H4B H 0.9668 0.9417 0.9111 0.066 Uiso 1 1 calc R
H4C H 0.9664 0.8461 0.8327 0.066 Uiso 1 1 calc R
C5 C 0.90400(10) 0.58809(19) 0.7603(3) 0.0302(6) Uani 1 1 d .
C6 C 0.86278(11) 0.5514(2) 0.8006(4) 0.0433(8) Uani 1 1 d .
H6A H 0.8650 0.5789 0.8818 0.065 Uiso 1 1 calc R
H6B H 0.8640 0.4812 0.8069 0.065 Uiso 1 1 calc R
H6C H 0.8333 0.5709 0.7387 0.065 Uiso 1 1 calc R
C7 C 0.95091(11) 0.5661(2) 0.8625(3) 0.0452(8) Uani 1 1 d .
H7A H 0.9508 0.5936 0.9418 0.068 Uiso 1 1 calc R
H7B H 0.9764 0.5942 0.8391 0.068 Uiso 1 1 calc R
H7C H 0.9552 0.4964 0.8714 0.068 Uiso 1 1 calc R
C8 C 0.90211(12) 0.5465(2) 0.6341(3) 0.0422(8) Uani 1 1 d .
H8A H 0.8720 0.5619 0.5719 0.063 Uiso 1 1 calc R
H8B H 0.9059 0.4766 0.6411 0.063 Uiso 1 1 calc R
H8C H 0.9272 0.5743 0.6085 0.063 Uiso 1 1 calc R
C9 C 0.71815(10) 0.53541(18) 0.5561(3) 0.0281(6) Uani 1 1 d .
H9 H 0.7006 0.5733 0.5943 0.034 Uiso 1 1 calc R
C10 C 0.71811(10) 0.43529(19) 0.5713(3) 0.0312(7) Uani 1 1 d .
H10 H 0.7018 0.4066 0.6206 0.037 Uiso 1 1 calc R
C11 C 0.74289(8) 0.37854(18) 0.5115(2) 0.0234(6) Uani 1 1 d .
C12 C 0.76670(10) 0.42370(19) 0.4384(3) 0.0287(6) Uani 1 1 d .
H12 H 0.7828 0.3870 0.3951 0.034 Uiso 1 1 calc R
C13 C 0.76579(10) 0.52471(18) 0.4318(3) 0.0267(6) Uani 1 1 d .
H13 H 0.7825 0.5552 0.3848 0.032 Uiso 1 1 calc R
C14 C 0.86301(10) 0.73751(19) 0.1470(3) 0.0322(7) Uani 1 1 d .
H14 H 0.8404 0.7380 0.0662 0.039 Uiso 1 1 calc R
C15 C 0.91029(10) 0.73731(18) 0.1546(3) 0.0287(6) Uani 1 1 d .
H15 H 0.9193 0.7381 0.0820 0.034 Uiso 1 1 calc R
C16 C 0.94396(10) 0.73584(18) 0.2760(3) 0.0292(6) Uani 1 1 d .
C17 C 0.92922(11) 0.7352(2) 0.3811(3) 0.0335(7) Uani 1 1 d .
H17 H 0.9513 0.7343 0.4626 0.040 Uiso 1 1 calc R
C18 C 0.88047(10) 0.7359(2) 0.3630(3) 0.0349(7) Uani 1 1 d .
H18 H 0.8706 0.7355 0.4342 0.042 Uiso 1 1 calc R
H1WA H 0.7313 0.7470 0.2620 0.080 Uiso 1 1 d D
H1WB H 0.7828 0.7456 0.2795 0.080 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'
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'
Mn Mn 0.3368 0.7283 '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
O1 Mn1 O1 180.00(4) . 7_666
O1 Mn1 O5 90.29(7) . 7_666
O1 Mn1 O5 89.71(7) 7_666 7_666
O1 Mn1 O5 89.71(7) . .
O1 Mn1 O5 90.29(7) 7_666 .
O5 Mn1 O5 180.0 7_666 .
O1 Mn1 N1 86.95(7) . .
O1 Mn1 N1 93.05(7) 7_666 .
O5 Mn1 N1 90.29(7) 7_666 .
O5 Mn1 N1 89.71(7) . .
O1 Mn1 N1 93.05(7) . 7_666
O1 Mn1 N1 86.95(7) 7_666 7_666
O5 Mn1 N1 89.71(7) 7_666 7_666
O5 Mn1 N1 90.29(7) . 7_666
N1 Mn1 N1 180.000(1) . 7_666
O2 P1 O1 116.75(11) . .
O2 P1 O4 111.25(11) . .
O1 P1 O4 109.93(10) . .
O2 P1 O3 113.27(10) . .
O1 P1 O3 104.23(11) . .
O4 P1 O3 99.93(10) . .
P1 O1 Mn1 129.85(11) . .
C1 O3 P1 128.55(18) . .
C5 O4 P1 126.84(16) . .
C9 N1 C13 117.0(2) . .
C9 N1 Mn1 120.13(16) . .
C13 N1 Mn1 122.34(17) . .
N2 N2 C11 112.5(3) 7_656 .
C14 N3 C18 116.6(3) . .
N4 N4 C16 113.8(3) 2_755 .
O3 C1 C2 104.0(2) . .
O3 C1 C4 111.5(2) . .
C2 C1 C4 111.3(2) . .
O3 C1 C3 108.5(2) . .
C2 C1 C3 110.1(3) . .
C4 C1 C3 111.1(3) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O4 C5 C8 108.0(2) . .
O4 C5 C7 104.0(2) . .
C8 C5 C7 111.8(2) . .
O4 C5 C6 111.1(2) . .
C8 C5 C6 111.3(3) . .
C7 C5 C6 110.4(3) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N1 C9 C10 123.6(2) . .
N1 C9 H9 118.2 . .
C10 C9 H9 118.2 . .
C9 C10 C11 118.4(3) . .
C9 C10 H10 120.8 . .
C11 C10 H10 120.8 . .
C10 C11 C12 119.3(2) . .
C10 C11 N2 114.7(2) . .
C12 C11 N2 126.0(2) . .
C13 C12 C11 118.1(2) . .
C13 C12 H12 121.0 . .
C11 C12 H12 121.0 . .
N1 C13 C12 123.5(2) . .
N1 C13 H13 118.2 . .
C12 C13 H13 118.2 . .
N3 C14 C15 125.1(3) . .
N3 C14 H14 117.4 . .
C15 C14 H14 117.4 . .
C14 C15 C16 117.1(3) . .
C14 C15 H15 121.4 . .
C16 C15 H15 121.4 . .
C17 C16 C15 119.7(3) . .
C17 C16 N4 117.0(3) . .
C15 C16 N4 123.3(3) . .
C16 C17 C18 118.8(3) . .
C16 C17 H17 120.6 . .
C18 C17 H17 120.6 . .
N3 C18 C17 122.8(3) . .
N3 C18 H18 118.6 . .
C17 C18 H18 118.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.1136(18) .
Mn1 O1 2.1136(18) 7_666
Mn1 O5 2.1882(19) 7_666
Mn1 O5 2.1882(19) .
Mn1 N1 2.313(2) .
Mn1 N1 2.313(2) 7_666
P1 O2 1.482(2) .
P1 O1 1.499(2) .
P1 O4 1.5875(19) .
P1 O3 1.5883(19) .
O3 C1 1.456(3) .
O4 C5 1.463(3) .
N1 C9 1.339(3) .
N1 C13 1.344(3) .
N2 N2 1.233(4) 7_656
N2 C11 1.446(3) .
N3 C14 1.341(4) .
N3 C18 1.349(4) .
N4 N4 1.230(5) 2_755
N4 C16 1.444(4) .
C1 C2 1.513(4) .
C1 C4 1.518(4) .
C1 C3 1.515(4) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 C8 1.499(4) .
C5 C7 1.516(4) .
C5 C6 1.522(4) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C10 1.377(4) .
C9 H9 0.9300 .
C10 C11 1.381(4) .
C10 H10 0.9300 .
C11 C12 1.386(4) .
C12 C13 1.380(4) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 C15 1.382(4) .
C14 H14 0.9300 .
C15 C16 1.395(4) .
C15 H15 0.9300 .
C16 C17 1.377(4) .
C17 C18 1.399(4) .
C17 H17 0.9300 .
C18 H18 0.9300 .
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 Mn1 29.90(18) .
O4 P1 O1 Mn1 157.82(13) .
O3 P1 O1 Mn1 -95.85(15) .
O1 Mn1 O1 P1 -150(100) 7_666
O5 Mn1 O1 P1 -34.89(15) 7_666
O5 Mn1 O1 P1 145.11(15) .
N1 Mn1 O1 P1 -125.16(15) .
N1 Mn1 O1 P1 54.84(15) 7_666
O2 P1 O3 C1 39.8(2) .
O1 P1 O3 C1 167.7(2) .
O4 P1 O3 C1 -78.6(2) .
O2 P1 O4 C5 80.5(2) .
O1 P1 O4 C5 -50.4(2) .
O3 P1 O4 C5 -159.6(2) .
O1 Mn1 N1 C9 116.3(2) .
O1 Mn1 N1 C9 -63.7(2) 7_666
O5 Mn1 N1 C9 26.0(2) 7_666
O5 Mn1 N1 C9 -154.0(2) .
N1 Mn1 N1 C9 165(100) 7_666
O1 Mn1 N1 C13 -54.7(2) .
O1 Mn1 N1 C13 125.3(2) 7_666
O5 Mn1 N1 C13 -145.0(2) 7_666
O5 Mn1 N1 C13 35.0(2) .
N1 Mn1 N1 C13 -6(100) 7_666
P1 O3 C1 C2 165.56(19) .
P1 O3 C1 C4 45.5(3) .
P1 O3 C1 C3 -77.2(3) .
P1 O4 C5 C8 88.3(3) .
P1 O4 C5 C7 -152.8(2) .
P1 O4 C5 C6 -34.1(3) .
C13 N1 C9 C10 2.2(4) .
Mn1 N1 C9 C10 -169.3(2) .
N1 C9 C10 C11 -2.0(4) .
C9 C10 C11 C12 -0.2(4) .
C9 C10 C11 N2 179.3(2) .
N2 N2 C11 C10 171.1(3) 7_656
N2 N2 C11 C12 -9.4(4) 7_656
C10 C11 C12 C13 2.0(4) .
N2 C11 C12 C13 -177.4(3) .
C9 N1 C13 C12 -0.2(4) .
Mn1 N1 C13 C12 171.1(2) .
C11 C12 C13 N1 -1.8(4) .
C18 N3 C14 C15 -0.3(4) .
N3 C14 C15 C16 0.5(4) .
C14 C15 C16 C17 -0.3(4) .
C14 C15 C16 N4 -179.8(2) .
N4 N4 C16 C17 179.57(17) 2_755
N4 N4 C16 C15 -0.9(3) 2_755
C15 C16 C17 C18 0.1(4) .
N4 C16 C17 C18 179.6(2) .
C14 N3 C18 C17 0.0(4) .
C16 C17 C18 N3 0.1(4) .
