#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:27:35 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180430 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/99/7209932.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_7209932
loop_
_publ_author_name
'Duan, Chunmei'
'Luo, Daibing'
'Shang, Rui'
'Lin, Zhien'
_publ_section_title
;
 Solvent-free synthesis of new manganese phosphate--oxalate hybrid solids
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5602
_journal_paper_doi               10.1039/c3ce40457a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C7 H7 Mn N O8 P'
_chemical_formula_weight         319.05
_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                92.040(7)
_cell_angle_beta                 95.790(8)
_cell_angle_gamma                107.914(8)
_cell_formula_units_Z            2
_cell_length_a                   6.1008(8)
_cell_length_b                   6.7115(7)
_cell_length_c                   12.9864(8)
_cell_measurement_reflns_used    1902
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9115
_cell_measurement_theta_min      3.1549
_cell_volume                     502.13(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω 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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3793
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92749
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0306
_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)+(0.0296P)²+0.1664P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                1504
_reflns_number_total             1764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40457a.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7209932
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
Mn1 Mn 0.27981(7) 0.09690(6) 0.46331(3) 0.01415(15) Uani 1 1 d .
P1 P 0.75057(12) 0.41651(11) 0.58924(6) 0.01344(19) Uani 1 1 d .
O1 O 0.6346(3) 0.2032(3) 0.53136(15) 0.0155(4) Uani 1 1 d .
O2 O 0.7606(3) 0.5958(3) 0.52152(15) 0.0161(4) Uani 1 1 d .
O3 O 0.6306(3) 0.4399(3) 0.68686(15) 0.0234(5) Uani 1 1 d .
H1 H 0.5336 0.3277 0.6950 0.035 Uiso 1 1 calc R
O4 O 1.0020(3) 0.4307(3) 0.63671(15) 0.0194(5) Uani 1 1 d .
H2 H 1.0801 0.4230 0.5898 0.029 Uiso 1 1 calc R
O5 O -0.0948(3) -0.0290(3) 0.39857(15) 0.0175(5) Uani 1 1 d .
O6 O 0.2807(3) 0.0840(3) 0.29869(15) 0.0204(5) Uani 1 1 d .
O7 O -0.3167(3) -0.1484(3) 0.24841(16) 0.0292(6) Uani 1 1 d .
O8 O 0.0618(4) 0.0247(4) 0.14692(16) 0.0333(6) Uani 1 1 d .
N1 N -0.5287(4) 0.2309(4) 0.08681(19) 0.0229(6) Uani 1 1 d .
H3 H -0.6586 0.1645 0.1082 0.027 Uiso 1 1 calc R
C1 C -0.1306(5) -0.0582(4) 0.3003(2) 0.0169(7) Uani 1 1 d .
C2 C 0.0890(5) 0.0244(4) 0.2431(2) 0.0183(7) Uani 1 1 d .
C3 C -0.3477(5) 0.3272(5) 0.1560(2) 0.0267(8) Uani 1 1 d .
H4 H -0.3622 0.3218 0.2265 0.032 Uiso 1 1 calc R
C4 C -0.1389(5) 0.4352(5) 0.1233(2) 0.0264(8) Uani 1 1 d .
H5 H -0.0133 0.5043 0.1720 0.032 Uiso 1 1 calc R
C5 C -0.1134(5) 0.4421(4) 0.0186(2) 0.0188(7) Uani 1 1 d .
C6 C -0.3074(5) 0.3379(5) -0.0508(2) 0.0243(7) Uani 1 1 d .
H6 H -0.2974 0.3381 -0.1218 0.029 Uiso 1 1 calc R
C7 C -0.5141(5) 0.2343(5) -0.0149(2) 0.0248(7) Uani 1 1 d .
H7 H -0.6440 0.1666 -0.0616 0.030 Uiso 1 1 calc R
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
O6 Mn1 O1 107.27(7) . .
O6 Mn1 O2 96.32(8) . 2_666
O1 Mn1 O2 93.70(7) . 2_666
O6 Mn1 O5 150.69(7) . 2_556
O1 Mn1 O5 101.66(7) . 2_556
O2 Mn1 O5 86.24(7) 2_666 2_556
O6 Mn1 O1 89.93(8) . 2_656
O1 Mn1 O1 78.17(7) . 2_656
O2 Mn1 O1 170.96(7) 2_666 2_656
O5 Mn1 O1 91.52(7) 2_556 2_656
O6 Mn1 O5 74.99(7) . .
O1 Mn1 O5 176.68(7) . .
O2 Mn1 O5 88.42(7) 2_666 .
O5 Mn1 O5 75.91(8) 2_556 .
O1 Mn1 O5 99.54(7) 2_656 .
O2 P1 O1 112.82(11) . .
O2 P1 O3 110.68(11) . .
O1 P1 O3 110.97(11) . .
O2 P1 O4 109.68(11) . .
O1 P1 O4 109.48(11) . .
O3 P1 O4 102.74(12) . .
P1 O1 Mn1 123.92(11) . .
P1 O1 Mn1 131.51(11) . 2_656
Mn1 O1 Mn1 101.83(7) . 2_656
P1 O2 Mn1 137.14(12) . 2_666
P1 O3 H1 109.5 . .
P1 O4 H2 109.5 . .
C1 O5 Mn1 140.71(17) . 2_556
C1 O5 Mn1 114.64(17) . .
Mn1 O5 Mn1 104.09(8) 2_556 .
C2 O6 Mn1 118.00(18) . .
C3 N1 C7 121.7(3) . .
C3 N1 H3 119.1 . .
C7 N1 H3 119.1 . .
O7 C1 O5 126.4(3) . .
O7 C1 C2 118.4(2) . .
O5 C1 C2 115.1(2) . .
O8 C2 O6 125.2(3) . .
O8 C2 C1 118.2(3) . .
O6 C2 C1 116.6(2) . .
N1 C3 C4 120.0(3) . .
N1 C3 H4 120.0 . .
C4 C3 H4 120.0 . .
C3 C4 C5 120.7(3) . .
C3 C4 H5 119.6 . .
C5 C4 H5 119.6 . .
C4 C5 C6 117.2(3) . .
C4 C5 C5 121.5(3) . 2_565
C6 C5 C5 121.3(3) . 2_565
C7 C6 C5 120.3(3) . .
C7 C6 H6 119.9 . .
C5 C6 H6 119.9 . .
N1 C7 C6 120.2(3) . .
N1 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O6 2.137(2) .
Mn1 O1 2.1433(19) .
Mn1 O2 2.1558(19) 2_666
Mn1 O5 2.2023(18) 2_556
Mn1 O1 2.2324(19) 2_656
Mn1 O5 2.240(2) .
P1 O2 1.5053(19) .
P1 O1 1.5193(19) .
P1 O3 1.553(2) .
P1 O4 1.568(2) .
O1 Mn1 2.2324(18) 2_656
O2 Mn1 2.1558(18) 2_666
O3 H1 0.8200 .
O4 H2 0.8200 .
O5 C1 1.270(3) .
O5 Mn1 2.2023(18) 2_556
O6 C2 1.253(3) .
O7 C1 1.226(3) .
O8 C2 1.244(3) .
N1 C3 1.328(4) .
N1 C7 1.333(4) .
N1 H3 0.8600 .
C1 C2 1.558(4) .
C3 C4 1.375(4) .
C3 H4 0.9300 .
C4 C5 1.385(4) .
C4 H5 0.9300 .
C5 C6 1.390(4) .
C5 C5 1.501(5) 2_565
C6 C7 1.376(4) .
C6 H6 0.9300 .
C7 H7 0.9300 .
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
N1 H3 O8 0.86 1.81 2.666(3) 177.3 1_455
