#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:56:51 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180405 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/74/7207453.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_7207453
loop_
_publ_author_name
'Zhang, Xiu-Tang'
'Fan, Li-Ming'
'Zhao, Xian'
'Sun, Di'
'Li, Da-Cheng'
'Dou, Jian-Min'
_publ_section_title
;
 Syntheses, crystal structures, and properties of five mixed-ligand
 coordination polymers based on novel
 quaterphenyl-2,5,2′,5′-tetracarboxylic acid ligand
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              2053
_journal_paper_doi               10.1039/c2ce06329h
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C23 H15 Mn N2 O5'
_chemical_formula_weight         454.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 99.314(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.749(2)
_cell_length_b                   12.010(2)
_cell_length_c                   14.524(3)
_cell_measurement_reflns_used    2817
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      47.406
_cell_measurement_theta_min      4.864
_cell_volume                     2022.4(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10880
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.9468
_exptl_absorpt_correction_T_min  0.9216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3551
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0884P)²+2.6302P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1735
_reflns_number_gt                2760
_reflns_number_total             3551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce06329h.txt
_cod_data_source_block           Mn
_cod_original_cell_volume        2022.3(6)
_cod_original_sg_symbol_H-M      p2(1)/n
_cod_database_code               7207453
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
C1 C -0.0630(4) 1.0327(3) 0.9179(3) 0.0446(12) Uani 1 1 d .
H1 H -0.1057 1.0559 0.8616 0.054 Uiso 1 1 calc R
C2 C -0.0107(4) 0.8927(3) 1.0310(3) 0.0437(11) Uani 1 1 d .
H2 H -0.0166 0.8205 1.0530 0.052 Uiso 1 1 calc R
C3 C -0.0760(3) 0.9243(3) 0.9473(3) 0.0326(9) Uani 1 1 d .
C4 C -0.1600(3) 0.8511(3) 0.8899(3) 0.0298(9) Uani 1 1 d .
C5 C -0.2672(3) 0.8959(3) 0.8517(3) 0.0326(9) Uani 1 1 d .
H5 H -0.2851 0.9679 0.8682 0.039 Uiso 1 1 calc R
C6 C -0.3471(3) 0.8374(3) 0.7906(3) 0.0293(8) Uani 1 1 d .
C7 C -0.3238(3) 0.7281(3) 0.7706(3) 0.0320(9) Uani 1 1 d .
H7 H -0.3767 0.6876 0.7290 0.038 Uiso 1 1 calc R
C8 C -0.2222(3) 0.6786(3) 0.8122(3) 0.0320(9) Uani 1 1 d .
H8 H -0.2095 0.6036 0.8016 0.038 Uiso 1 1 calc R
C9 C -0.1382(3) 0.7400(3) 0.8699(3) 0.0286(8) Uani 1 1 d .
C10 C -0.4554(4) 0.8940(4) 0.7458(3) 0.0359(9) Uani 1 1 d .
C11 C -0.0218(3) 0.6869(3) 0.9001(3) 0.0338(9) Uani 1 1 d .
C12 C 0.2472(5) 0.2339(5) 0.8938(4) 0.0594(14) Uani 1 1 d .
H12 H 0.1814 0.2183 0.8509 0.071 Uiso 1 1 calc R
C13 C 0.3370(6) 0.1568(5) 0.9054(5) 0.0746(18) Uani 1 1 d .
H13 H 0.3311 0.0915 0.8705 0.090 Uiso 1 1 calc R
C14 C 0.4332(6) 0.1781(6) 0.9682(5) 0.0769(19) Uani 1 1 d .
H14 H 0.4931 0.1266 0.9773 0.092 Uiso 1 1 calc R
C15 C 0.4427(4) 0.2760(5) 1.0187(4) 0.0583(15) Uani 1 1 d .
C16 C 0.3481(4) 0.3509(4) 1.0025(3) 0.0417(11) Uani 1 1 d .
C17 C 0.3550(3) 0.4543(4) 1.0517(3) 0.0398(11) Uani 1 1 d .
C18 C 0.4543(4) 0.4826(5) 1.1141(3) 0.0531(13) Uani 1 1 d .
C19 C 0.5476(4) 0.4046(7) 1.1292(4) 0.0737(19) Uani 1 1 d .
H19 H 0.6137 0.4222 1.1711 0.088 Uiso 1 1 calc R
C20 C 0.5418(5) 0.3075(7) 1.0846(5) 0.077(2) Uani 1 1 d .
H20 H 0.6038 0.2586 1.0965 0.093 Uiso 1 1 calc R
C21 C 0.4558(5) 0.5866(6) 1.1576(3) 0.0699(18) Uani 1 1 d .
H21 H 0.5205 0.6086 1.1992 0.084 Uiso 1 1 calc R
C22 C 0.3641(5) 0.6550(6) 1.1398(4) 0.0664(17) Uani 1 1 d .
H22 H 0.3651 0.7242 1.1687 0.080 Uiso 1 1 calc R
C23 C 0.2682(4) 0.6209(4) 1.0776(3) 0.0517(12) Uani 1 1 d .
H23 H 0.2054 0.6689 1.0657 0.062 Uiso 1 1 calc R
Mn1 Mn 0.10925(5) 0.45727(5) 0.93658(4) 0.0324(2) Uani 1 1 d .
N1 N 0.2614(3) 0.5243(3) 1.0347(2) 0.0380(8) Uani 1 1 d .
N2 N 0.2513(3) 0.3283(3) 0.9412(2) 0.0410(9) Uani 1 1 d .
O1 O -0.0180(2) 0.5959(2) 0.94720(18) 0.0343(6) Uani 1 1 d .
O2 O 0.0627(3) 0.7301(3) 0.8749(3) 0.0587(10) Uani 1 1 d .
O3 O -0.4995(3) 0.8619(2) 0.66470(19) 0.0405(7) Uani 1 1 d .
O4 O -0.4929(3) 0.9707(3) 0.7898(3) 0.0723(12) Uani 1 1 d .
O5 O 0.1729(3) 0.5484(3) 0.8221(2) 0.0471(8) Uani 1 1 d D
H1W H 0.125(4) 0.525(4) 0.779(3) 0.09(2) Uiso 1 1 d D
H2W H 0.160(5) 0.6135(18) 0.834(4) 0.09(2) 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'
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
C2 C1 C3 122.4(4) 3_577 . ?
C2 C1 H1 118.8 3_577 . ?
C3 C1 H1 118.8 . . ?
C1 C2 C3 120.4(4) 3_577 . ?
C1 C2 H2 119.8 3_577 . ?
C3 C2 H2 119.8 . . ?
C2 C3 C1 117.2(4) . . ?
C2 C3 C4 124.0(4) . . ?
C1 C3 C4 118.8(3) . . ?
C9 C4 C5 117.9(3) . . ?
C9 C4 C3 123.9(3) . . ?
C5 C4 C3 118.2(3) . . ?
C6 C5 C4 122.4(4) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C7 118.9(4) . . ?
C5 C6 C10 119.4(4) . . ?
C7 C6 C10 121.6(3) . . ?
C8 C7 C6 120.2(4) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 120.8(4) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C4 119.5(3) . . ?
C8 C9 C11 118.1(3) . . ?
C4 C9 C11 122.1(3) . . ?
O4 C10 O3 125.3(4) . . ?
O4 C10 C6 117.5(3) . . ?
O3 C10 C6 117.1(4) . . ?
O2 C11 O1 124.0(4) . . ?
O2 C11 C9 118.2(4) . . ?
O1 C11 C9 117.7(3) . . ?
N2 C12 C13 122.9(6) . . ?
N2 C12 H12 118.5 . . ?
C13 C12 H12 118.5 . . ?
C14 C13 C12 119.2(6) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 120.3(5) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C16 117.3(5) . . ?
C14 C15 C20 124.5(6) . . ?
C16 C15 C20 118.2(6) . . ?
N2 C16 C15 122.2(5) . . ?
N2 C16 C17 118.5(4) . . ?
C15 C16 C17 119.3(5) . . ?
N1 C17 C18 121.8(5) . . ?
N1 C17 C16 117.6(4) . . ?
C18 C17 C16 120.6(4) . . ?
C17 C18 C21 117.2(5) . . ?
C17 C18 C19 118.6(6) . . ?
C21 C18 C19 124.2(5) . . ?
C20 C19 C18 121.4(5) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C15 121.9(5) . . ?
C19 C20 H20 119.0 . . ?
C15 C20 H20 119.0 . . ?
C22 C21 C18 120.5(5) . . ?
C22 C21 H21 119.7 . . ?
C18 C21 H21 119.7 . . ?
C21 C22 C23 119.0(5) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
N1 C23 C22 123.4(5) . . ?
N1 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
O3 Mn1 O5 89.29(12) 2_446 . y
O3 Mn1 O1 93.30(11) 2_446 3_567 y
O5 Mn1 O1 165.47(12) . 3_567 y
O3 Mn1 N1 164.22(13) 2_446 . y
O5 Mn1 N1 88.19(13) . . y
O1 Mn1 N1 93.04(12) 3_567 . ?
O3 Mn1 O1 96.34(11) 2_446 . y
O5 Mn1 O1 89.68(12) . . y
O1 Mn1 O1 75.82(10) 3_567 . ?
N1 Mn1 O1 99.22(12) . . ?
O3 Mn1 N2 90.76(13) 2_446 . ?
O5 Mn1 N2 91.38(13) . . ?
O1 Mn1 N2 102.86(11) 3_567 . ?
N1 Mn1 N2 73.74(13) . . ?
O1 Mn1 N2 172.84(12) . . ?
C23 N1 C17 118.1(4) . . ?
C23 N1 Mn1 126.7(3) . . ?
C17 N1 Mn1 115.2(3) . . ?
C12 N2 C16 118.1(4) . . ?
C12 N2 Mn1 127.2(3) . . ?
C16 N2 Mn1 114.7(3) . . ?
C11 O1 Mn1 131.7(3) . 3_567 ?
C11 O1 Mn1 123.8(3) . . ?
Mn1 O1 Mn1 104.18(10) 3_567 . ?
C10 O3 Mn1 126.1(3) . 2_456 ?
Mn1 O5 H1W 97(5) . . ?
Mn1 O5 H2W 102(5) . . ?
H1W O5 H2W 112(2) . . ?
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
C1 C2 1.377(6) 3_577 ?
C1 C3 1.386(6) . ?
C1 H1 0.9300 . ?
C2 C1 1.377(6) 3_577 ?
C2 C3 1.381(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.475(5) . ?
C4 C9 1.398(5) . ?
C4 C5 1.399(5) . ?
C5 C6 1.376(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.382(5) . ?
C6 C10 1.497(5) . ?
C7 C8 1.382(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.397(5) . ?
C8 H8 0.9300 . ?
C9 C11 1.508(5) . ?
C10 O4 1.240(5) . ?
C10 O3 1.268(5) . ?
C11 O2 1.228(5) . ?
C11 O1 1.286(5) . ?
C12 N2 1.323(6) . ?
C12 C13 1.394(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.357(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.380(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.419(6) . ?
C15 C20 1.433(9) . ?
C16 N2 1.354(6) . ?
C16 C17 1.428(7) . ?
C17 N1 1.374(6) . ?
C17 C18 1.399(6) . ?
C18 C21 1.399(9) . ?
C18 C19 1.431(9) . ?
C19 C20 1.331(9) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.346(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.387(7) . ?
C22 H22 0.9300 . ?
C23 N1 1.313(6) . ?
C23 H23 0.9300 . ?
Mn1 O3 2.127(3) 2_446 y
Mn1 O5 2.219(3) . y
Mn1 O1 2.234(3) 3_567 y
Mn1 N1 2.247(3) . y
Mn1 O1 2.259(3) . y
Mn1 N2 2.270(4) . y
O1 Mn1 2.234(3) 3_567 ?
O3 Mn1 2.127(3) 2_456 ?
O5 H1W 0.8200(11) . ?
O5 H2W 0.8201(11) . ?
