#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179732 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/28/7002809.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_7002809
loop_
_publ_author_name
'Fu, Ruibiao'
'Hu, Shengmin'
'Wu, Xintao'
_publ_section_title
;
 Syntheses, crystal structures, thermal stabilities, luminescence and
 magnetism of two 3D pillared metal phosphonates
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              9843
_journal_page_last               9848
_journal_paper_doi               10.1039/b907619k
_journal_year                    2009
_chemical_formula_sum            'C19 H16 Mn3 N3 O12 P2'
_chemical_formula_weight         705.11
_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                106.843(3)
_cell_angle_beta                 97.861(2)
_cell_angle_gamma                100.576(3)
_cell_formula_units_Z            2
_cell_length_a                   8.652(3)
_cell_length_b                   10.293(3)
_cell_length_c                   14.164(4)
_cell_measurement_reflns_used    2715
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.1280
_cell_volume                     1162.3(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9018
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6209
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.6000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.0500
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0510P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                4164
_reflns_number_total             5242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907619k.txt
_cod_data_source_block           f1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002809
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
Mn1 Mn 0.50234(3) 0.24997(3) 0.492470(19) 0.01512(9) Uani 1 1 d . . .
Mn2 Mn 1.10024(3) 0.22290(3) 0.602373(18) 0.01241(9) Uani 1 1 d . . .
Mn3 Mn 0.89808(3) 0.27355(3) 0.397821(18) 0.01248(9) Uani 1 1 d . . .
P1 P 0.73986(5) 0.54011(5) 0.48886(3) 0.01042(11) Uani 1 1 d . . .
P2 P 0.73716(5) 0.03582(5) 0.48653(3) 0.01031(11) Uani 1 1 d . . .
O1 O 0.59395(14) 0.58016(13) 0.44555(9) 0.0154(3) Uani 1 1 d . . .
O2 O 1.10539(14) 0.38231(13) 0.53176(9) 0.0139(3) Uani 1 1 d . . .
O3 O 0.72487(14) 0.38212(13) 0.45668(9) 0.0134(3) Uani 1 1 d . . .
O4 O 1.06388(15) 0.40825(14) 0.33598(9) 0.0156(3) Uani 1 1 d . . .
H2 H 1.069(3) 0.497(3) 0.3404(17) 0.028(6) Uiso 1 1 d . . .
O5 O 0.65479(15) 0.79968(14) 0.65236(9) 0.0178(3) Uani 1 1 d . . .
O6 O 1.07761(15) 0.15877(13) 0.32291(9) 0.0155(3) Uani 1 1 d . . .
O7 O 0.59262(14) 0.07457(13) 0.43999(9) 0.0151(3) Uani 1 1 d . . .
O8 O 0.27678(14) 0.12174(13) 0.54162(9) 0.0136(3) Uani 1 1 d . . .
O9 O 0.89344(14) 0.11223(13) 0.46622(9) 0.0145(3) Uani 1 1 d . . .
O10 O 0.92907(15) 0.09047(15) 0.66322(9) 0.0154(3) Uani 1 1 d . . .
H4 H 0.920(3) 0.004(3) 0.6613(19) 0.036(7) Uiso 1 1 d . . .
O11 O 0.65411(15) 0.30023(14) 0.64048(9) 0.0171(3) Uani 1 1 d . . .
O12 O 0.92134(14) 0.34011(13) 0.67421(9) 0.0161(3) Uani 1 1 d . . .
N1 N 1.25452(19) 0.3204(2) 0.75753(12) 0.0245(4) Uani 1 1 d . . .
N2 N 0.7272(2) 0.16492(19) 0.24958(12) 0.0237(4) Uani 1 1 d . . .
N3 N 0.8661(4) 0.2958(4) -0.0287(2) 0.0841(10) Uani 1 1 d . . .
C1 C 0.7786(2) 0.60596(19) 0.62770(12) 0.0124(3) Uani 1 1 d . . .
H1 H 0.700(2) 0.563(2) 0.6529(15) 0.014(5) Uiso 1 1 d . . .
C2 C 0.7841(2) 0.76104(19) 0.65623(12) 0.0127(3) Uani 1 1 d . . .
C3 C 0.7732(2) 0.10578(19) 0.62496(12) 0.0119(3) Uani 1 1 d . . .
H3 H 0.686(2) 0.065(2) 0.6504(14) 0.011(5) Uiso 1 1 d . . .
C4 C 0.7824(2) 0.26076(19) 0.65058(12) 0.0118(3) Uani 1 1 d . . .
C5 C 1.4112(3) 0.3464(4) 0.77298(17) 0.0650(11) Uani 1 1 d . . .
H5 H 1.452(3) 0.316(3) 0.718(2) 0.073(9) Uiso 1 1 d . . .
C6 C 1.5117(3) 0.4161(4) 0.86575(17) 0.0665(11) Uani 1 1 d . . .
H6 H 1.627(4) 0.440(4) 0.872(3) 0.110(13) Uiso 1 1 d . . .
C7 C 1.4486(2) 0.4617(2) 0.94925(14) 0.0241(5) Uani 1 1 d . . .
C8 C 1.2846(3) 0.4294(4) 0.93390(16) 0.0523(8) Uani 1 1 d . . .
H7 H 1.238(4) 0.457(3) 0.992(2) 0.082(10) Uiso 1 1 d . . .
C9 C 1.1929(3) 0.3591(3) 0.83892(16) 0.0484(8) Uani 1 1 d . . .
H8 H 1.072(4) 0.323(4) 0.826(3) 0.106(12) Uiso 1 1 d . . .
C10 C 0.6411(4) 0.2314(3) 0.20321(19) 0.0525(8) Uani 1 1 d . . .
H9 H 0.639(4) 0.326(4) 0.242(2) 0.082(11) Uiso 1 1 d . . .
C11 C 0.5524(4) 0.1708(3) 0.1064(2) 0.0598(9) Uani 1 1 d . . .
H20 H 0.494(4) 0.227(3) 0.080(2) 0.071(9) Uiso 1 1 d . . .
C12 C 0.5464(3) 0.0343(2) 0.05270(14) 0.0268(5) Uani 1 1 d . . .
C13 C 0.6326(3) -0.0347(3) 0.10215(18) 0.0453(7) Uani 1 1 d . . .
H21 H 0.634(3) -0.129(3) 0.067(2) 0.066(9) Uiso 1 1 d . . .
C14 C 0.7201(3) 0.0335(3) 0.19900(18) 0.0436(6) Uani 1 1 d . . .
H22 H 0.791(3) -0.019(3) 0.2298(19) 0.059(8) Uiso 1 1 d . . .
C15 C 0.9588(5) 0.3001(5) 0.0563(3) 0.0852(12) Uani 1 1 d . . .
H23 H 0.983(5) 0.402(5) 0.112(3) 0.125(15) Uiso 1 1 d . . .
C16 C 1.0109(5) 0.1890(4) 0.0709(3) 0.0726(10) Uani 1 1 d . . .
H24 H 1.081(4) 0.200(4) 0.135(2) 0.090(12) Uiso 1 1 d . . .
C17 C 0.9726(3) 0.0617(3) -0.00594(19) 0.0553(8) Uani 1 1 d . . .
C18 C 0.8757(5) 0.0580(5) -0.0939(2) 0.0738(11) Uani 1 1 d . . .
H25 H 0.842(4) -0.028(4) -0.146(3) 0.099(13) Uiso 1 1 d . . .
C19 C 0.8265(5) 0.1742(5) -0.1007(3) 0.0839(12) Uani 1 1 d . . .
H26 H 0.762(4) 0.169(4) -0.166(3) 0.105(13) 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'
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
_geom_angle_publ_flag
O7 Mn1 O1 175.30(4) . 2_666 ?
O7 Mn1 O5 91.19(5) . 2_666 ?
O1 Mn1 O5 91.33(5) 2_666 2_666 ?
O7 Mn1 O11 89.85(5) . . ?
O1 Mn1 O11 87.53(5) 2_666 . ?
O5 Mn1 O11 178.23(4) 2_666 . ?
O7 Mn1 O3 88.30(5) . . ?
O1 Mn1 O3 95.36(5) 2_666 . ?
O5 Mn1 O3 96.46(5) 2_666 . ?
O11 Mn1 O3 85.00(5) . . ?
O7 Mn1 O8 93.48(5) . . ?
O1 Mn1 O8 82.70(5) 2_666 . ?
O5 Mn1 O8 86.89(5) 2_666 . ?
O11 Mn1 O8 91.61(5) . . ?
O3 Mn1 O8 176.17(4) . . ?
O8 Mn2 O2 101.39(5) 1_655 . ?
O8 Mn2 N1 93.73(6) 1_655 . ?
O2 Mn2 N1 107.91(6) . . ?
O8 Mn2 O10 113.43(5) 1_655 . ?
O2 Mn2 O10 140.06(5) . . ?
N1 Mn2 O10 89.31(6) . . ?
O8 Mn2 O9 96.83(5) 1_655 . ?
O2 Mn2 O9 79.70(5) . . ?
N1 Mn2 O9 165.52(5) . . ?
O10 Mn2 O9 77.41(5) . . ?
O8 Mn2 O12 176.95(5) 1_655 . ?
O2 Mn2 O12 78.38(5) . . ?
N1 Mn2 O12 83.49(6) . . ?
O10 Mn2 O12 67.86(5) . . ?
O9 Mn2 O12 86.13(5) . . ?
O3 Mn3 O9 104.39(5) . . ?
O3 Mn3 N2 91.20(6) . . ?
O9 Mn3 N2 103.06(6) . . ?
O3 Mn3 O4 109.82(5) . . ?
O9 Mn3 O4 141.17(5) . . ?
N2 Mn3 O4 94.17(6) . . ?
O3 Mn3 O2 97.25(5) . . ?
O9 Mn3 O2 80.18(5) . . ?
N2 Mn3 O2 169.94(5) . . ?
O4 Mn3 O2 77.85(5) . . ?
O3 Mn3 O6 175.66(4) . . ?
O9 Mn3 O6 79.01(5) . . ?
N2 Mn3 O6 85.35(6) . . ?
O4 Mn3 O6 67.89(5) . . ?
O2 Mn3 O6 85.95(5) . . ?
O1 P1 O3 113.47(7) . . ?
O1 P1 O2 111.79(7) . 2_766 ?
O3 P1 O2 111.79(7) . 2_766 ?
O1 P1 C1 110.35(8) . . ?
O3 P1 C1 107.59(8) . . ?
O2 P1 C1 101.05(8) 2_766 . ?
O7 P2 O8 114.05(7) . 2_656 ?
O7 P2 O9 111.47(7) . . ?
O8 P2 O9 111.88(7) 2_656 . ?
O7 P2 C3 110.65(7) . . ?
O8 P2 C3 107.00(8) 2_656 . ?
O9 P2 C3 100.90(7) . . ?
P1 O1 Mn1 129.23(8) . 2_666 ?
P1 O2 Mn2 123.10(7) 2_766 . ?
P1 O2 Mn3 116.92(7) 2_766 . ?
Mn2 O2 Mn3 100.28(5) . . ?
P1 O3 Mn3 126.64(7) . . ?
P1 O3 Mn1 115.90(7) . . ?
Mn3 O3 Mn1 117.09(6) . . ?
C1 O4 Mn3 104.51(10) 2_766 . ?
C2 O5 Mn1 119.28(11) . 2_666 ?
C2 O6 Mn3 111.26(11) 2_766 . ?
P2 O7 Mn1 129.57(8) . . ?
P2 O8 Mn2 123.81(7) 2_656 1_455 ?
P2 O8 Mn1 114.73(6) 2_656 . ?
Mn2 O8 Mn1 121.04(6) 1_455 . ?
P2 O9 Mn3 122.12(7) . . ?
P2 O9 Mn2 116.72(7) . . ?
Mn3 O9 Mn2 99.83(5) . . ?
C3 O10 Mn2 104.60(10) . . ?
C4 O11 Mn1 121.30(11) . . ?
C4 O12 Mn2 110.62(11) . . ?
C5 N1 C9 115.65(19) . . ?
C5 N1 Mn2 122.14(14) . . ?
C9 N1 Mn2 122.18(14) . . ?
C14 N2 C10 116.4(2) . . ?
C14 N2 Mn3 120.68(15) . . ?
C10 N2 Mn3 122.57(16) . . ?
C19 N3 C15 115.4(4) . . ?
O4 C1 C2 107.54(14) 2_766 . ?
O4 C1 P1 107.59(11) 2_766 . ?
C2 C1 P1 105.91(11) . . ?
O5 C2 O6 125.06(17) . 2_766 ?
O5 C2 C1 119.05(16) . . ?
O6 C2 C1 115.77(15) 2_766 . ?
O10 C3 C4 107.30(14) . . ?
O10 C3 P2 107.40(11) . . ?
C4 C3 P2 105.91(11) . . ?
O11 C4 O12 124.83(17) . . ?
O11 C4 C3 118.54(16) . . ?
O12 C4 C3 116.44(15) . . ?
N1 C5 C6 124.4(2) . . ?
C7 C6 C5 120.1(2) . . ?
C6 C7 C8 115.6(2) . . ?
C6 C7 C7 122.3(2) . 2_867 ?
C8 C7 C7 122.1(2) . 2_867 ?
C7 C8 C9 120.7(2) . . ?
N1 C9 C8 123.5(2) . . ?
N2 C10 C11 123.1(3) . . ?
C12 C11 C10 120.7(2) . . ?
C13 C12 C11 115.8(2) . . ?
C13 C12 C12 121.9(3) . 2_655 ?
C11 C12 C12 122.3(3) . 2_655 ?
C12 C13 C14 120.2(2) . . ?
N2 C14 C13 123.8(2) . . ?
N3 C15 C16 124.3(4) . . ?
C15 C16 C17 120.4(3) . . ?
C16 C17 C18 114.9(3) . . ?
C16 C17 C17 122.5(3) . 2_755 ?
C18 C17 C17 122.6(4) . 2_755 ?
C19 C18 C17 120.4(4) . . ?
N3 C19 C18 124.6(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O7 2.0786(14) . ?
Mn1 O1 2.0898(14) 2_666 ?
Mn1 O5 2.1661(14) 2_666 ?
Mn1 O11 2.1807(14) . ?
Mn1 O3 2.3492(13) . ?
Mn1 O8 2.4481(13) . ?
Mn2 O8 2.1405(13) 1_655 ?
Mn2 O2 2.1520(13) . ?
Mn2 N1 2.2464(17) . ?
Mn2 O10 2.2544(14) . ?
Mn2 O9 2.2918(13) . ?
Mn2 O12 2.3003(13) . ?
Mn3 O3 2.1462(13) . ?
Mn3 O9 2.1485(13) . ?
Mn3 N2 2.2423(17) . ?
Mn3 O4 2.2505(14) . ?
Mn3 O2 2.2739(13) . ?
Mn3 O6 2.3091(13) . ?
P1 O1 1.5052(13) . ?
P1 O3 1.5317(14) . ?
P1 O2 1.5379(13) 2_766 ?
P1 C1 1.8446(18) . ?
P2 O7 1.5057(13) . ?
P2 O8 1.5310(14) 2_656 ?
P2 O9 1.5416(13) . ?
P2 C3 1.8419(18) . ?
O1 Mn1 2.0898(14) 2_666 ?
O2 P1 1.5379(12) 2_766 ?
O4 C1 1.438(2) 2_766 ?
O5 C2 1.254(2) . ?
O5 Mn1 2.1661(14) 2_666 ?
O6 C2 1.264(2) 2_766 ?
O8 P2 1.5310(14) 2_656 ?
O8 Mn2 2.1405(13) 1_455 ?
O10 C3 1.437(2) . ?
O11 C4 1.254(2) . ?
O12 C4 1.263(2) . ?
N1 C5 1.307(3) . ?
N1 C9 1.324(3) . ?
N2 C14 1.321(3) . ?
N2 C10 1.330(3) . ?
N3 C19 1.316(5) . ?
N3 C15 1.336(5) . ?
C1 O4 1.438(2) 2_766 ?
C1 C2 1.519(3) . ?
C2 O6 1.264(2) 2_766 ?
C3 C4 1.514(3) . ?
C5 C6 1.382(3) . ?
C6 C7 1.366(3) . ?
C7 C8 1.368(3) . ?
C7 C7 1.488(4) 2_867 ?
C8 C9 1.377(3) . ?
C10 C11 1.378(3) . ?
C11 C12 1.378(3) . ?
C12 C13 1.376(3) . ?
C12 C12 1.492(4) 2_655 ?
C13 C14 1.382(3) . ?
C15 C16 1.362(5) . ?
C16 C17 1.389(5) . ?
C17 C18 1.390(4) . ?
C17 C17 1.480(6) 2_755 ?
C18 C19 1.365(6) . ?
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
O4 H2 O12 0.89(3) 1.74(3) 2.617(2) 170(2) 2_766
O10 H4 O6 0.87(3) 1.75(3) 2.620(2) 171(2) 2_756
