#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:13:32 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180417 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/86/7208652.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_7208652
loop_
_publ_author_name
'Deng, Zhao-Peng'
'Zhang, Zhu-Yan'
'Huo, Li-Hua'
'Ng, Seik Weng'
'Zhao, Hui'
'Gao, Shan'
_publ_section_title
;
 Syntheses, crystal structures and properties of transition metal
 coordination polymers based on isophthalic acid and flexible bis(pyridyl)
 ligand with unsymmetrical spacer: influence of metal cations, ligand
 conformations and coordination modes
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6548
_journal_paper_doi               10.1039/c2ce25339a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C19 H17 Mn N3 O5, C H4 O'
_chemical_formula_sum            'C20 H21 Mn N3 O6'
_chemical_formula_weight         454.34
_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                99.96(3)
_cell_angle_beta                 110.61(3)
_cell_angle_gamma                106.37(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0247(18)
_cell_length_b                   10.475(2)
_cell_length_c                   12.242(2)
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.24
_cell_volume                     990.4(5)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9771
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.9071
_exptl_absorpt_correction_T_min  0.8828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4473
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0454
_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)+(0.0567P)²+0.7730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                3255
_reflns_number_total             4473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25339a.txt
_cod_data_source_block           complex5
_cod_database_code               7208652
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 0.55704(6) 0.21343(4) 0.16593(4) 0.02864(15) Uani 1 1 d .
O1 O 0.4981(3) 0.40768(19) 0.2065(2) 0.0353(5) Uani 1 1 d .
O1W O 0.6883(3) 0.2565(2) 0.3665(2) 0.0402(5) Uani 1 1 d D
H1W1 H 0.687(4) 0.337(2) 0.392(3) 0.060 Uiso 1 1 d D
H1W2 H 0.787(2) 0.257(3) 0.407(3) 0.060 Uiso 1 1 d D
O2 O 0.6644(4) 0.5002(3) 0.4075(2) 0.0646(8) Uani 1 1 d .
O3 O 0.6206(3) 1.03089(19) 0.1439(2) 0.0373(5) Uani 1 1 d .
O4 O 0.5641(3) 0.81990(19) 0.02604(19) 0.0343(5) Uani 1 1 d .
O5 O 0.0171(4) 0.2590(3) 0.4806(3) 0.0690(8) Uani 1 1 d D
H5O H 0.108(4) 0.332(4) 0.515(5) 0.103 Uiso 1 1 d D
N1 N 0.3093(3) 0.0953(2) 0.1685(2) 0.0332(6) Uani 1 1 d .
N2 N -0.1541(4) -0.3587(3) 0.0179(3) 0.0454(7) Uani 1 1 d D
H2N H -0.256(2) -0.390(4) -0.040(3) 0.054 Uiso 1 1 d D
N3 N -0.2063(3) -0.6286(3) 0.1709(3) 0.0362(6) Uani 1 1 d .
C1 C 0.5725(4) 0.5050(3) 0.3050(3) 0.0347(7) Uani 1 1 d .
C2 C 0.5539(4) 0.6442(3) 0.3051(3) 0.0290(6) Uani 1 1 d .
C3 C 0.5638(4) 0.7026(3) 0.2133(3) 0.0282(6) Uani 1 1 d .
H3 H 0.5702 0.6515 0.1461 0.034 Uiso 1 1 calc R
C4 C 0.5643(4) 0.8376(3) 0.2206(3) 0.0304(6) Uani 1 1 d .
C5 C 0.5490(5) 0.9103(3) 0.3191(3) 0.0410(8) Uani 1 1 d .
H5 H 0.5499 1.0003 0.3252 0.049 Uiso 1 1 calc R
C6 C 0.5325(5) 0.8504(3) 0.4089(3) 0.0465(9) Uani 1 1 d .
H6 H 0.5171 0.8984 0.4728 0.056 Uiso 1 1 calc R
C7 C 0.5390(4) 0.7187(3) 0.4030(3) 0.0371(7) Uani 1 1 d .
H7 H 0.5332 0.6804 0.4651 0.044 Uiso 1 1 calc R
C8 C 0.5835(4) 0.9012(3) 0.1222(3) 0.0292(6) Uani 1 1 d .
C9 C 0.2139(4) -0.0324(3) 0.0895(3) 0.0320(6) Uani 1 1 d .
H9 H 0.2482 -0.0648 0.0304 0.038 Uiso 1 1 calc R
C10 C 0.0667(4) -0.1199(3) 0.0901(3) 0.0335(7) Uani 1 1 d .
C11 C 0.0158(5) -0.0701(3) 0.1766(3) 0.0446(8) Uani 1 1 d .
H11 H -0.0821 -0.1254 0.1802 0.054 Uiso 1 1 calc R
C12 C 0.1107(5) 0.0625(4) 0.2583(4) 0.0495(9) Uani 1 1 d .
H12 H 0.0765 0.0982 0.3163 0.059 Uiso 1 1 calc R
C13 C 0.2573(4) 0.1414(3) 0.2524(3) 0.0415(8) Uani 1 1 d .
H13 H 0.3225 0.2298 0.3086 0.050 Uiso 1 1 calc R
C14 C -0.0268(4) -0.2593(3) -0.0022(3) 0.0371(7) Uani 1 1 d .
H14A H -0.0819 -0.2468 -0.0812 0.044 Uiso 1 1 calc R
H14B H 0.0559 -0.2996 -0.0073 0.044 Uiso 1 1 calc R
C15 C -0.2343(4) -0.5479(3) 0.0984(3) 0.0324(6) Uani 1 1 d .
H15 H -0.3463 -0.5680 0.0443 0.039 Uiso 1 1 calc R
C16 C -0.1065(4) -0.4353(3) 0.0984(3) 0.0340(7) Uani 1 1 d .
C17 C 0.0599(4) -0.4069(3) 0.1792(3) 0.0429(8) Uani 1 1 d .
H17 H 0.1499 -0.3338 0.1822 0.051 Uiso 1 1 calc R
C18 C 0.0898(4) -0.4892(4) 0.2553(4) 0.0491(9) Uani 1 1 d .
H18 H 0.2004 -0.4707 0.3111 0.059 Uiso 1 1 calc R
C19 C -0.0447(4) -0.5989(4) 0.2482(3) 0.0442(8) Uani 1 1 d .
H19 H -0.0222 -0.6542 0.2990 0.053 Uiso 1 1 calc R
C20 C 0.0046(7) 0.1864(6) 0.5647(5) 0.0880(16) Uani 1 1 d .
H20A H 0.0758 0.1325 0.5718 0.132 Uiso 1 1 calc R
H20B H -0.1116 0.1252 0.5370 0.132 Uiso 1 1 calc R
H20C H 0.0410 0.2517 0.6432 0.132 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'
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 O3 93.54(9) 2_665 1_545
O4 Mn1 O1W 177.82(8) 2_665 .
O3 Mn1 O1W 87.96(9) 1_545 .
O4 Mn1 N1 91.64(10) 2_665 .
O3 Mn1 N1 92.31(9) 1_545 .
O1W Mn1 N1 89.88(10) . .
O4 Mn1 O1 91.34(8) 2_665 .
O3 Mn1 O1 175.08(8) 1_545 .
O1W Mn1 O1 87.18(9) . .
N1 Mn1 O1 86.90(9) . .
O4 Mn1 N3 88.45(10) 2_665 1_665
O3 Mn1 N3 99.24(9) 1_545 1_665
O1W Mn1 N3 89.74(10) . 1_665
N1 Mn1 N3 168.42(9) . 1_665
O1 Mn1 N3 81.52(9) . 1_665
C1 O1 Mn1 126.4(2) . .
Mn1 O1W H1W1 101(3) . .
Mn1 O1W H1W2 127(3) . .
H1W1 O1W H1W2 108.9(16) . .
C8 O3 Mn1 152.1(2) . 1_565
C8 O4 Mn1 137.38(19) . 2_665
C20 O5 H5O 110(4) . .
C9 N1 C13 117.4(3) . .
C9 N1 Mn1 119.1(2) . .
C13 N1 Mn1 123.3(2) . .
C16 N2 C14 120.4(3) . .
C16 N2 H2N 120(3) . .
C14 N2 H2N 115(3) . .
C15 N3 C19 117.4(3) . .
C15 N3 Mn1 115.9(2) . 1_445
C19 N3 Mn1 126.3(2) . 1_445
O1 C1 O2 126.4(3) . .
O1 C1 C2 118.9(3) . .
O2 C1 C2 114.8(3) . .
C7 C2 C3 119.5(2) . .
C7 C2 C1 119.2(3) . .
C3 C2 C1 121.1(3) . .
C2 C3 C4 120.8(3) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C5 C4 C3 118.8(3) . .
C5 C4 C8 121.5(2) . .
C3 C4 C8 119.7(3) . .
C4 C5 C6 120.6(3) . .
C4 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C7 C6 C5 119.8(3) . .
C7 C6 H6 120.1 . .
C5 C6 H6 120.1 . .
C2 C7 C6 120.3(3) . .
C2 C7 H7 119.8 . .
C6 C7 H7 119.8 . .
O4 C8 O3 125.3(3) . .
O4 C8 C4 116.7(2) . .
O3 C8 C4 118.0(3) . .
N1 C9 C10 124.0(3) . .
N1 C9 H9 118.0 . .
C10 C9 H9 118.0 . .
C11 C10 C9 117.5(3) . .
C11 C10 C14 124.0(3) . .
C9 C10 C14 118.5(3) . .
C10 C11 C12 119.7(3) . .
C10 C11 H11 120.1 . .
C12 C11 H11 120.1 . .
C11 C12 C13 118.8(3) . .
C11 C12 H12 120.6 . .
C13 C12 H12 120.6 . .
N1 C13 C12 122.5(3) . .
N1 C13 H13 118.7 . .
C12 C13 H13 118.7 . .
N2 C14 C10 116.9(3) . .
N2 C14 H14A 108.1 . .
C10 C14 H14A 108.1 . .
N2 C14 H14B 108.1 . .
C10 C14 H14B 108.1 . .
H14A C14 H14B 107.3 . .
N3 C15 C16 124.4(3) . .
N3 C15 H15 117.8 . .
C16 C15 H15 117.8 . .
C17 C16 C15 117.1(3) . .
C17 C16 N2 124.5(3) . .
C15 C16 N2 118.4(3) . .
C18 C17 C16 118.8(3) . .
C18 C17 H17 120.6 . .
C16 C17 H17 120.6 . .
C19 C18 C17 119.9(3) . .
C19 C18 H18 120.0 . .
C17 C18 H18 120.0 . .
N3 C19 C18 122.4(3) . .
N3 C19 H19 118.8 . .
C18 C19 H19 118.8 . .
O5 C20 H20A 109.5 . .
O5 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
O5 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O4 2.129(2) 2_665
Mn1 O3 2.146(2) 1_545
Mn1 O1W 2.214(2) .
Mn1 N1 2.244(3) .
Mn1 O1 2.262(2) .
Mn1 N3 2.277(3) 1_665
O1 C1 1.250(4) .
O1W H1W1 0.85(3) .
O1W H1W2 0.86(4) .
O2 C1 1.256(4) .
O3 C8 1.259(3) .
O3 Mn1 2.146(2) 1_565
O4 C8 1.252(4) .
O4 Mn1 2.129(2) 2_665
O5 C20 1.399(5) .
O5 H5O 0.86(5) .
N1 C9 1.336(4) .
N1 C13 1.343(4) .
N2 C16 1.403(4) .
N2 C14 1.442(4) .
N2 H2N 0.86(4) .
N3 C15 1.338(4) .
N3 C19 1.338(4) .
N3 Mn1 2.277(3) 1_445
C1 C2 1.515(4) .
C2 C7 1.383(4) .
C2 C3 1.386(4) .
C3 C4 1.400(4) .
C3 H3 0.9300 .
C4 C5 1.383(4) .
C4 C8 1.511(4) .
C5 C6 1.388(5) .
C5 H5 0.9300 .
C6 C7 1.387(4) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C9 C10 1.389(4) .
C9 H9 0.9300 .
C10 C11 1.375(5) .
C10 C14 1.478(4) .
C11 C12 1.382(5) .
C11 H11 0.9300 .
C12 C13 1.383(5) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.398(4) .
C15 H15 0.9300 .
C16 C17 1.387(5) .
C17 C18 1.384(5) .
C17 H17 0.9300 .
C18 C19 1.381(5) .
C18 H18 0.9300 .
C19 H19 0.9300 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
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
N2 H2N O1 0.86(4) 2.340(16) 3.172(4) 162(3) 2
O1W H1W1 O2 0.85(3) 1.766(13) 2.599(3) 166(4) .
O1W H1W2 O5 0.86(4) 1.941(12) 2.790(4) 173(4) 1_655
O5 H5O O2 0.86(5) 2.052(12) 2.906(5) 176(6) 2_666
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
O4 Mn1 O1 C1 -159.1(3) 2_665
O1W Mn1 O1 C1 19.3(3) .
N1 Mn1 O1 C1 109.3(3) .
N3 Mn1 O1 C1 -70.9(3) 1_665
O4 Mn1 N1 C9 51.8(2) 2_665
O3 Mn1 N1 C9 -41.9(2) 1_545
O1W Mn1 N1 C9 -129.8(2) .
O1 Mn1 N1 C9 143.0(2) .
N3 Mn1 N1 C9 142.1(4) 1_665
O4 Mn1 N1 C13 -133.9(3) 2_665
O3 Mn1 N1 C13 132.5(3) 1_545
O1W Mn1 N1 C13 44.6(3) .
O1 Mn1 N1 C13 -42.6(3) .
N3 Mn1 N1 C13 -43.6(6) 1_665
Mn1 O1 C1 O2 -18.0(5) .
Mn1 O1 C1 C2 162.0(2) .
O1 C1 C2 C7 141.4(3) .
O2 C1 C2 C7 -38.6(4) .
O1 C1 C2 C3 -43.3(4) .
O2 C1 C2 C3 136.7(3) .
C7 C2 C3 C4 2.0(4) .
C1 C2 C3 C4 -173.3(3) .
C2 C3 C4 C5 -2.1(4) .
C2 C3 C4 C8 177.2(3) .
C3 C4 C5 C6 -0.4(5) .
C8 C4 C5 C6 -179.6(3) .
C4 C5 C6 C7 2.9(6) .
C3 C2 C7 C6 0.6(5) .
C1 C2 C7 C6 175.9(3) .
C5 C6 C7 C2 -3.0(6) .
Mn1 O4 C8 O3 -43.5(5) 2_665
Mn1 O4 C8 C4 137.9(2) 2_665
Mn1 O3 C8 O4 107.5(5) 1_565
Mn1 O3 C8 C4 -73.9(5) 1_565
C5 C4 C8 O4 -166.9(3) .
C3 C4 C8 O4 13.8(4) .
C5 C4 C8 O3 14.4(4) .
C3 C4 C8 O3 -164.8(3) .
C13 N1 C9 C10 -0.8(5) .
Mn1 N1 C9 C10 173.9(2) .
N1 C9 C10 C11 1.0(5) .
N1 C9 C10 C14 -179.7(3) .
C9 C10 C11 C12 0.0(5) .
C14 C10 C11 C12 -179.2(3) .
C10 C11 C12 C13 -1.2(6) .
C9 N1 C13 C12 -0.5(5) .
Mn1 N1 C13 C12 -174.9(3) .
C11 C12 C13 N1 1.5(6) .
C16 N2 C14 C10 -81.4(4) .
C11 C10 C14 N2 -14.8(5) .
C9 C10 C14 N2 166.0(3) .
C19 N3 C15 C16 -0.1(5) .
Mn1 N3 C15 C16 172.8(2) 1_445
N3 C15 C16 C17 0.2(5) .
N3 C15 C16 N2 -179.6(3) .
C14 N2 C16 C17 11.9(5) .
C14 N2 C16 C15 -168.4(3) .
C15 C16 C17 C18 -0.7(5) .
N2 C16 C17 C18 179.0(3) .
C16 C17 C18 C19 1.2(6) .
C15 N3 C19 C18 0.5(5) .
Mn1 N3 C19 C18 -171.5(3) 1_445
C17 C18 C19 N3 -1.1(6) .
