#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:32:27 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180477 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/46/7214627.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_7214627
loop_
_publ_author_name
'Duan, Chunmei'
'Luo, Daibing'
'Zeng, Hongmei'
'Kang, Maoping'
'Lin, Zhien'
_publ_section_title
;
 Solvent-free synthesis of new open-framework oxalate structures
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              5734
_journal_paper_doi               10.1039/c2ce25856k
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C9 H22 Mn2 N2 O17 P2'
_chemical_formula_weight         602.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.6900(6)
_cell_length_b                   14.4331(8)
_cell_length_c                   29.8442(8)
_cell_measurement_reflns_used    6545
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2003
_cell_measurement_theta_min      2.8707
_cell_volume                     4173.9(4)
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15127
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.451
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            light-pink
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0382
_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)+(0.0358P)²+4.6541P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                3115
_reflns_number_total             3680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25856k.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7214627
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.13053(4) 0.23551(4) 0.700512(15) 0.02466(14) Uani 1 1 d .
Mn2 Mn 0.24975(4) 0.45728(4) 0.546064(15) 0.02920(15) Uani 1 1 d .
P1 P 0.06314(8) 0.29612(7) 0.59580(3) 0.0264(2) Uani 1 1 d .
P2 P 0.28638(8) 0.53050(7) 0.65278(3) 0.0294(2) Uani 1 1 d .
O1 O 0.3254(3) 0.5029(3) 0.60690(8) 0.0786(12) Uani 1 1 d .
O2 O 0.3939(2) 0.49025(19) 0.68610(8) 0.0440(7) Uani 1 1 d .
H1 H 0.3713 0.4375 0.6932 0.066 Uiso 1 1 calc R
O3 O 0.1427(2) 0.49169(18) 0.66564(8) 0.0390(6) Uani 1 1 d .
H2 H 0.1363 0.4379 0.6570 0.058 Uiso 1 1 calc R
O4 O 0.2817(3) 0.6326(2) 0.65879(10) 0.0603(9) Uani 1 1 d .
O5 O 0.1881(2) 0.3217(2) 0.56932(8) 0.0402(6) Uani 1 1 d .
O6 O 0.0759(2) 0.32026(17) 0.64442(7) 0.0315(5) Uani 1 1 d .
O7 O -0.0689(2) 0.34434(19) 0.57759(8) 0.0410(6) Uani 1 1 d .
H3 H -0.0496 0.3968 0.5691 0.061 Uiso 1 1 calc R
O8 O 0.0284(2) 0.19072(19) 0.58922(8) 0.0431(7) Uani 1 1 d .
H4 H 0.0741 0.1597 0.6068 0.065 Uiso 1 1 calc R
O9 O 0.4461(2) 0.39624(19) 0.52473(8) 0.0417(7) Uani 1 1 d .
O10 O 0.6449(2) 0.4318(2) 0.49199(8) 0.0405(7) Uani 1 1 d .
O11 O 0.1305(2) 0.42305(18) 0.48493(7) 0.0338(6) Uani 1 1 d .
O12 O -0.0680(2) 0.45352(18) 0.45081(7) 0.0312(6) Uani 1 1 d .
O13 O -0.0729(2) 0.17063(17) 0.70349(7) 0.0308(6) Uani 1 1 d .
O14 O 0.0157(2) 0.31810(18) 0.75027(8) 0.0373(6) Uani 1 1 d .
O15 O -0.2684(2) 0.1722(2) 0.74166(8) 0.0439(7) Uani 1 1 d .
O16 O -0.1780(2) 0.31753(17) 0.78965(7) 0.0328(6) Uani 1 1 d .
N1 N -0.5559(4) 0.2255(3) 0.58343(17) 0.0941(18) Uani 1 1 d .
H5 H -0.6285 0.2630 0.5818 0.141 Uiso 1 1 calc R
H6 H -0.5845 0.1676 0.5879 0.141 Uiso 1 1 calc R
H7 H -0.5084 0.2284 0.5579 0.141 Uiso 1 1 calc R
N2 N -0.2439(3) 0.0468(2) 0.65545(9) 0.0347(7) Uani 1 1 d .
H2B H -0.1819 0.0851 0.6689 0.042 Uiso 1 1 calc R
C1 C 0.5260(3) 0.4502(3) 0.50465(10) 0.0318(8) Uani 1 1 d .
C2 C 0.0187(3) 0.4642(2) 0.48163(9) 0.0241(7) Uani 1 1 d .
C3 C -0.1511(3) 0.2020(2) 0.73337(10) 0.0258(7) Uani 1 1 d .
C4 C -0.0986(3) 0.2865(2) 0.76006(10) 0.0252(7) Uani 1 1 d .
C5 C -0.4702(5) 0.2531(3) 0.61948(14) 0.0550(12) Uani 1 1 d .
H8 H -0.5234 0.2508 0.6470 0.066 Uiso 1 1 calc R
H9 H -0.4420 0.3168 0.6148 0.066 Uiso 1 1 calc R
C6 C -0.3431(4) 0.1939(3) 0.62498(15) 0.0530(11) Uani 1 1 d .
H10 H -0.3023 0.1834 0.5957 0.064 Uiso 1 1 calc R
H11 H -0.2763 0.2273 0.6430 0.064 Uiso 1 1 calc R
C7 C -0.3719(3) 0.1018(3) 0.64670(12) 0.0367(9) Uani 1 1 d .
H12 H -0.4196 0.1121 0.6748 0.044 Uiso 1 1 calc R
H13 H -0.4326 0.0661 0.6274 0.044 Uiso 1 1 calc R
C8 C -0.2720(5) -0.0306(3) 0.68683(15) 0.0567(12) Uani 1 1 d .
H14 H -0.3133 -0.0067 0.7137 0.085 Uiso 1 1 calc R
H15 H -0.1871 -0.0613 0.6941 0.085 Uiso 1 1 calc R
H16 H -0.3340 -0.0739 0.6730 0.085 Uiso 1 1 calc R
C9 C -0.1801(4) 0.0122(3) 0.61348(13) 0.0503(11) Uani 1 1 d .
H17 H -0.0977 -0.0218 0.6205 0.076 Uiso 1 1 calc R
H18 H -0.1573 0.0637 0.5945 0.076 Uiso 1 1 calc R
H19 H -0.2439 -0.0277 0.5982 0.076 Uiso 1 1 calc R
OW1 O -0.2346(4) 0.2758(2) 0.52024(12) 0.0901(13) Uani 1 1 d .
H20 H -0.3029 0.2201 0.5096 0.108 Uiso 1 1 d R
H21 H -0.2805 0.3247 0.5075 0.108 Uiso 1 1 d 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
O4 Mn1 O6 92.30(10) 8_655 .
O4 Mn1 O13 94.91(10) 8_655 .
O6 Mn1 O13 93.08(9) . .
O4 Mn1 O15 89.49(12) 8_655 6_657
O6 Mn1 O15 165.49(9) . 6_657
O13 Mn1 O15 101.11(9) . 6_657
O4 Mn1 O14 168.00(10) 8_655 .
O6 Mn1 O14 95.34(9) . .
O13 Mn1 O14 75.47(8) . .
O15 Mn1 O14 85.43(10) 6_657 .
O4 Mn1 O16 96.67(11) 8_655 6_657
O6 Mn1 O16 90.32(8) . 6_657
O13 Mn1 O16 167.79(9) . 6_657
O15 Mn1 O16 75.18(8) 6_657 6_657
O14 Mn1 O16 92.54(9) . 6_657
O1 Mn2 O5 96.01(13) . .
O1 Mn2 O12 93.49(11) . 5_566
O5 Mn2 O12 107.28(9) . 5_566
O1 Mn2 O9 94.32(11) . .
O5 Mn2 O9 88.24(9) . .
O12 Mn2 O9 161.77(9) 5_566 .
O1 Mn2 O10 93.24(12) . 5_666
O5 Mn2 O10 161.43(9) . 5_666
O12 Mn2 O10 88.14(9) 5_566 5_666
O9 Mn2 O10 75.00(9) . 5_666
O1 Mn2 O11 168.52(11) . .
O5 Mn2 O11 85.32(10) . .
O12 Mn2 O11 75.28(8) 5_566 .
O9 Mn2 O11 97.12(9) . .
O10 Mn2 O11 88.82(9) 5_666 .
O5 P1 O6 112.87(14) . .
O5 P1 O7 111.85(14) . .
O6 P1 O7 107.60(14) . .
O5 P1 O8 110.32(15) . .
O6 P1 O8 111.36(14) . .
O7 P1 O8 102.33(14) . .
O1 P2 O4 112.8(2) . .
O1 P2 O3 111.28(15) . .
O4 P2 O3 107.56(17) . .
O1 P2 O2 108.73(18) . .
O4 P2 O2 108.32(15) . .
O3 P2 O2 108.00(14) . .
P2 O1 Mn2 144.16(16) . .
P2 O2 H1 109.5 . .
P2 O3 H2 109.5 . .
P2 O4 Mn1 139.03(16) . 8_665
P1 O5 Mn2 128.22(15) . .
P1 O6 Mn1 130.21(15) . .
P1 O7 H3 109.5 . .
P1 O8 H4 109.5 . .
C1 O9 Mn2 115.2(2) . .
C1 O10 Mn2 115.4(2) . 5_666
C2 O11 Mn2 114.48(19) . .
C2 O12 Mn2 115.8(2) . 5_566
C3 O13 Mn1 114.8(2) . .
C4 O14 Mn1 114.4(2) . .
C3 O15 Mn1 115.0(2) . 6_557
C4 O16 Mn1 114.6(2) . 6_557
C5 N1 H5 109.5 . .
C5 N1 H6 109.5 . .
H5 N1 H6 109.5 . .
C5 N1 H7 109.5 . .
H5 N1 H7 109.5 . .
H6 N1 H7 109.5 . .
C8 N2 C9 110.9(3) . .
C8 N2 C7 110.9(3) . .
C9 N2 C7 112.1(3) . .
C8 N2 H2B 107.5 . .
C9 N2 H2B 107.5 . .
C7 N2 H2B 107.5 . .
O10 C1 O9 125.9(4) . .
O10 C1 C1 116.5(4) . 5_666
O9 C1 C1 117.6(3) . 5_666
O11 C2 O12 125.7(3) . .
O11 C2 C2 117.9(3) . 5_566
O12 C2 C2 116.4(3) . 5_566
O15 C3 O13 124.8(3) . .
O15 C3 C4 118.3(3) . .
O13 C3 C4 116.9(3) . .
O14 C4 O16 125.9(3) . .
O14 C4 C3 117.8(3) . .
O16 C4 C3 116.3(3) . .
N1 C5 C6 113.7(4) . .
N1 C5 H8 108.8 . .
C6 C5 H8 108.8 . .
N1 C5 H9 108.8 . .
C6 C5 H9 108.8 . .
H8 C5 H9 107.7 . .
C7 C6 C5 113.3(3) . .
C7 C6 H10 108.9 . .
C5 C6 H10 108.9 . .
C7 C6 H11 108.9 . .
C5 C6 H11 108.9 . .
H10 C6 H11 107.7 . .
N2 C7 C6 113.0(3) . .
N2 C7 H12 109.0 . .
C6 C7 H12 109.0 . .
N2 C7 H13 109.0 . .
C6 C7 H13 109.0 . .
H12 C7 H13 107.8 . .
N2 C8 H14 109.5 . .
N2 C8 H15 109.5 . .
H14 C8 H15 109.5 . .
N2 C8 H16 109.5 . .
H14 C8 H16 109.5 . .
H15 C8 H16 109.5 . .
N2 C9 H17 109.5 . .
N2 C9 H18 109.5 . .
H17 C9 H18 109.5 . .
N2 C9 H19 109.5 . .
H17 C9 H19 109.5 . .
H18 C9 H19 109.5 . .
H20 OW1 H21 98.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O4 2.116(3) 8_655
Mn1 O6 2.140(2) .
Mn1 O13 2.184(2) .
Mn1 O15 2.185(2) 6_657
Mn1 O14 2.205(2) .
Mn1 O16 2.220(2) 6_657
Mn2 O1 2.066(3) .
Mn2 O5 2.161(3) .
Mn2 O12 2.184(2) 5_566
Mn2 O9 2.191(2) .
Mn2 O10 2.213(3) 5_666
Mn2 O11 2.215(2) .
P1 O5 1.492(2) .
P1 O6 1.497(2) .
P1 O7 1.555(2) .
P1 O8 1.570(3) .
P2 O1 1.475(3) .
P2 O4 1.486(3) .
P2 O3 1.549(2) .
P2 O2 1.553(2) .
O2 H1 0.8200 .
O3 H2 0.8200 .
O4 Mn1 2.116(3) 8_665
O7 H3 0.8200 .
O8 H4 0.8200 .
O9 C1 1.252(4) .
O10 C1 1.242(4) .
O10 Mn2 2.213(3) 5_666
O11 C2 1.240(4) .
O12 C2 1.255(3) .
O12 Mn2 2.184(2) 5_566
O13 C3 1.255(4) .
O14 C4 1.233(4) .
O15 C3 1.240(4) .
O15 Mn1 2.185(2) 6_557
O16 C4 1.253(4) .
O16 Mn1 2.220(2) 6_557
N1 C5 1.416(5) .
N1 H5 0.8900 .
N1 H6 0.8900 .
N1 H7 0.8900 .
N2 C8 1.483(5) .
N2 C9 1.483(5) .
N2 C7 1.496(4) .
N2 H2B 0.9100 .
C1 C1 1.547(7) 5_666
C2 C2 1.549(6) 5_566
C3 C4 1.544(5) .
C5 C6 1.508(6) .
C5 H8 0.9700 .
C5 H9 0.9700 .
C6 C7 1.506(6) .
C6 H10 0.9700 .
C6 H11 0.9700 .
C7 H12 0.9700 .
C7 H13 0.9700 .
C8 H14 0.9600 .
C8 H15 0.9600 .
C8 H16 0.9600 .
C9 H17 0.9600 .
C9 H18 0.9600 .
C9 H19 0.9600 .
OW1 H20 1.0885 .
OW1 H21 0.9168 .
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
O2 H1 O16 0.82 1.87 2.688(4) 178.9 6_657
O3 H2 O6 0.82 1.84 2.635(4) 164.7 .
O8 H4 O4 0.82 2.12 2.898(4) 157.4 8_655
N1 H5 O5 0.89 2.00 2.874(4) 165.8 1_455
N1 H6 O12 0.89 2.10 2.781(5) 132.4 4_456
N2 H2B O13 0.91 1.92 2.828(4) 171.4 .
OW1 H20 O11 1.09 2.17 3.158(4) 149.6 4_456
OW1 H21 O10 0.92 1.77 2.672(4) 168.5 1_455
