#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:47:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179128 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/90/4309053.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_4309053
loop_
_publ_author_name
'Yuan-Zhu Zhang'
'Song Gao'
'Zhe-Ming Wang'
'Gang Su'
'Hao-Ling Sun'
'Feng Pan'
_publ_contact_author_address
;
State Key Lab of Rare Earth Materials Chemistry and Applications &
PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry,
College of Chemistry and Molecular Engineering,
Peking University,
Beijing 100871,
China
;
_publ_contact_author_email       gaosong@pku.edu.cn
_publ_contact_author_fax         86-(10)-62751708
_publ_contact_author_name        'Prof. Song Gao'
_publ_contact_author_phone       86-(10)-62756320
_publ_section_title
;
Rational Synthesis and Magnetic Properties of a Family of Low-Dimensional
Heterometallic Cr-Mn Complexes Based on the Versatile Building Block
[Cr(2,2'-bipyridine)(CN)4]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4534
_journal_page_last               4545
_journal_paper_doi               10.1021/ic0484194
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C26 H20 Cr Mn N11 O2'
_chemical_formula_weight         625.47
_chemical_name_common            CrMn-dca
_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                 109.4386(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8628(4)
_cell_length_b                   7.9593(2)
_cell_length_c                   22.5123(8)
_cell_measurement_reflns_used    33307
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     2849.28(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.1149
_diffrn_reflns_av_sigmaI/netI    0.1331
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42532
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6513
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                2639
_reflns_number_total             6513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0484194si20041117_040813_5.cif
_cod_data_source_block           4
_cod_database_code               4309053
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 1.15352(3) 1.29755(7) -0.07385(3) 0.03154(19) Uani 1 1 d . . .
Mn1 Mn 1.33775(3) 0.79873(6) 0.07207(3) 0.03174(18) Uani 1 1 d . . .
N1 N 1.25538(18) 1.5928(4) 0.01845(16) 0.0396(9) Uani 1 1 d . . .
N2 N 1.26773(18) 1.0007(4) 0.00551(16) 0.0427(9) Uani 1 1 d . . .
N3 N 1.0720(2) 1.0116(4) -0.17620(18) 0.0657(11) Uani 1 1 d . . .
N4 N 1.2715(2) 1.3810(4) -0.15647(18) 0.0601(11) Uani 1 1 d . . .
N5 N 1.07157(16) 1.2600(3) -0.02357(16) 0.0321(8) Uani 1 1 d . . .
N6 N 1.05426(17) 1.4537(3) -0.12125(15) 0.0345(8) Uani 1 1 d . . .
N7 N 1.42805(17) 0.7622(3) 0.01972(16) 0.0318(8) Uani 1 1 d . . .
N8 N 1.44974(19) 0.9652(4) 0.11773(16) 0.0410(9) Uani 1 1 d . . .
N9 N 1.2657(2) 0.8616(4) 0.13295(19) 0.0608(11) Uani 1 1 d . . .
N10 N 1.1657(3) 0.9387(7) 0.1826(2) 0.115(2) Uani 1 1 d . . .
N11 N 1.1708(3) 0.9140(7) 0.2906(2) 0.1155(19) Uani 1 1 d . . .
C1 C 1.2188(2) 1.4854(5) -0.01232(19) 0.0342(10) Uani 1 1 d . . .
C2 C 1.2314(2) 1.1108(5) -0.02261(18) 0.0352(10) Uani 1 1 d . . .
C3 C 1.0991(2) 1.1097(5) -0.1378(2) 0.0420(11) Uani 1 1 d . . .
C4 C 1.2288(2) 1.3521(4) -0.12738(19) 0.0393(10) Uani 1 1 d . . .
C5 C 1.0873(2) 1.1777(4) 0.03116(19) 0.0378(10) Uani 1 1 d . . .
H5 H 1.1416 1.1385 0.0516 0.045 Uiso 1 1 calc R . .
C6 C 1.0266(2) 1.1488(4) 0.0584(2) 0.0419(11) Uani 1 1 d . . .
H6 H 1.0400 1.0933 0.0969 0.050 Uiso 1 1 calc R . .
C7 C 0.9458(2) 1.2028(5) 0.0281(2) 0.0441(11) Uani 1 1 d . . .
H7 H 0.9034 1.1816 0.0450 0.053 Uiso 1 1 calc R . .
C8 C 0.9289(2) 1.2897(5) -0.0282(2) 0.0420(11) Uani 1 1 d . . .
H8 H 0.8748 1.3280 -0.0493 0.050 Uiso 1 1 calc R . .
C9 C 0.9923(2) 1.3193(4) -0.05274(19) 0.0334(10) Uani 1 1 d . . .
C10 C 0.9828(2) 1.4246(4) -0.1083(2) 0.0380(10) Uani 1 1 d . . .
C11 C 0.9067(2) 1.4967(5) -0.1442(2) 0.0506(12) Uani 1 1 d . . .
H11 H 0.8572 1.4711 -0.1364 0.061 Uiso 1 1 calc R . .
C12 C 0.9062(3) 1.6070(5) -0.1916(2) 0.0584(13) Uani 1 1 d . . .
H12 H 0.8562 1.6575 -0.2158 0.070 Uiso 1 1 calc R . .
C13 C 0.9790(3) 1.6423(5) -0.2031(2) 0.0524(12) Uani 1 1 d . . .
H13 H 0.9791 1.7187 -0.2343 0.063 Uiso 1 1 calc R . .
C14 C 1.0524(3) 1.5629(4) -0.16775(19) 0.0422(11) Uani 1 1 d . . .
H14 H 1.1018 1.5851 -0.1761 0.051 Uiso 1 1 calc R . .
C15 C 1.4125(2) 0.6752(5) -0.0340(2) 0.0410(11) Uani 1 1 d . . .
H15 H 1.3581 0.6366 -0.0541 0.049 Uiso 1 1 calc R . .
C16 C 1.4729(3) 0.6403(4) -0.0607(2) 0.0482(12) Uani 1 1 d . . .
H16 H 1.4596 0.5797 -0.0980 0.058 Uiso 1 1 calc R . .
C17 C 1.5531(3) 0.6966(5) -0.0311(2) 0.0546(13) Uani 1 1 d . . .
H17 H 1.5956 0.6734 -0.0477 0.066 Uiso 1 1 calc R . .
C18 C 1.5699(2) 0.7873(5) 0.0232(2) 0.0505(12) Uani 1 1 d . . .
H18 H 1.6241 0.8268 0.0436 0.061 Uiso 1 1 calc R . .
C19 C 1.5070(2) 0.8205(4) 0.0477(2) 0.0361(10) Uani 1 1 d . . .
C20 C 1.5191(2) 0.9282(5) 0.1039(2) 0.0393(11) Uani 1 1 d . . .
C21 C 1.5969(3) 0.9947(6) 0.1392(2) 0.0600(14) Uani 1 1 d . . .
H21 H 1.6450 0.9660 0.1300 0.072 Uiso 1 1 calc R . .
C22 C 1.6018(3) 1.1036(6) 0.1878(3) 0.0748(17) Uani 1 1 d . . .
H22 H 1.6536 1.1466 0.2124 0.090 Uiso 1 1 calc R . .
C23 C 1.5308(4) 1.1480(5) 0.1997(2) 0.0686(15) Uani 1 1 d . . .
H23 H 1.5325 1.2259 0.2309 0.082 Uiso 1 1 calc R . .
C24 C 1.4557(3) 1.0739(5) 0.1640(2) 0.0551(13) Uani 1 1 d . . .
H24 H 1.4072 1.1015 0.1727 0.066 Uiso 1 1 calc R . .
C25 C 1.2227(3) 0.8956(6) 0.1602(2) 0.0539(12) Uani 1 1 d . . .
C26 C 1.1727(3) 0.9247(7) 0.2410(3) 0.0744(16) Uani 1 1 d . . .
O1 O 1.40951(15) 0.6045(3) 0.13924(13) 0.0506(8) Uani 1 1 d D . .
O2 O 1.42006(18) 1.3918(5) -0.20355(15) 0.0718(9) Uani 1 1 d D . .
H1A H 1.3798(17) 0.532(4) 0.1566(17) 0.070(7) Uiso 1 1 d D . .
H1B H 1.4669(11) 0.592(4) 0.1608(16) 0.070(7) Uiso 1 1 d D . .
H2A H 1.3751(18) 1.380(5) -0.1906(16) 0.070(7) Uiso 1 1 d D . .
H2B H 1.410(2) 1.414(5) -0.2441(10) 0.070(7) 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'
Cr Cr 0.3209 0.6236 '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'
O O 0.0106 0.0060 '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 Cr1 C4 94.44(14) . . ?
C2 Cr1 C3 85.44(15) . . ?
C4 Cr1 C3 87.83(15) . . ?
C2 Cr1 N6 167.05(13) . . ?
C4 Cr1 N6 96.96(13) . . ?
C3 Cr1 N6 88.87(13) . . ?
C2 Cr1 N5 90.39(13) . . ?
C4 Cr1 N5 175.14(12) . . ?
C3 Cr1 N5 93.09(13) . . ?
N6 Cr1 N5 78.30(12) . . ?
C2 Cr1 C1 92.75(13) . . ?
C4 Cr1 C1 86.91(14) . . ?
C3 Cr1 C1 174.29(14) . . ?
N6 Cr1 C1 93.97(12) . . ?
N5 Cr1 C1 92.34(12) . . ?
N9 Mn1 O1 91.33(12) . . ?
N9 Mn1 N1 97.63(12) . 1_545 ?
O1 Mn1 N1 87.53(11) . 1_545 ?
N9 Mn1 N7 170.53(13) . . ?
O1 Mn1 N7 87.47(10) . . ?
N1 Mn1 N7 91.71(11) 1_545 . ?
N9 Mn1 N2 88.61(12) . . ?
O1 Mn1 N2 178.41(12) . . ?
N1 Mn1 N2 94.05(10) 1_545 . ?
N7 Mn1 N2 92.33(11) . . ?
N9 Mn1 N8 97.85(13) . . ?
O1 Mn1 N8 85.10(10) . . ?
N1 Mn1 N8 163.00(12) 1_545 . ?
N7 Mn1 N8 72.69(12) . . ?
N2 Mn1 N8 93.33(11) . . ?
C1 N1 Mn1 173.0(3) . 1_565 ?
C2 N2 Mn1 172.7(3) . . ?
C5 N5 C9 118.3(3) . . ?
C5 N5 Cr1 127.3(2) . . ?
C9 N5 Cr1 114.3(3) . . ?
C10 N6 C14 119.0(3) . . ?
C10 N6 Cr1 114.3(3) . . ?
C14 N6 Cr1 126.2(3) . . ?
C15 N7 C19 117.7(3) . . ?
C15 N7 Mn1 125.5(2) . . ?
C19 N7 Mn1 116.6(3) . . ?
C24 N8 C20 118.7(4) . . ?
C24 N8 Mn1 124.9(3) . . ?
C20 N8 Mn1 115.4(3) . . ?
C25 N9 Mn1 174.3(4) . . ?
C25 N10 C26 123.9(5) . . ?
N1 C1 Cr1 175.9(3) . . ?
N2 C2 Cr1 173.7(3) . . ?
N3 C3 Cr1 174.6(4) . . ?
N4 C4 Cr1 179.0(4) . . ?
N5 C5 C6 122.8(3) . . ?
N5 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C7 C6 C5 119.2(4) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C8 118.6(4) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 H7 120.7 . . ?
C9 C8 C7 120.1(4) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
N5 C9 C8 121.0(4) . . ?
N5 C9 C10 114.7(3) . . ?
C8 C9 C10 124.1(4) . . ?
N6 C10 C11 121.3(4) . . ?
N6 C10 C9 115.4(3) . . ?
C11 C10 C9 123.2(4) . . ?
C12 C11 C10 118.5(4) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C13 C12 C11 120.3(4) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 119.1(4) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
N6 C14 C13 121.7(4) . . ?
N6 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
N7 C15 C16 123.3(4) . . ?
N7 C15 H15 118.4 . . ?
C16 C15 H15 118.4 . . ?
C17 C16 C15 118.6(4) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C18 C17 C16 119.0(4) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 120.2(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
N7 C19 C18 121.2(4) . . ?
N7 C19 C20 115.5(3) . . ?
C18 C19 C20 123.2(4) . . ?
N8 C20 C21 120.9(4) . . ?
N8 C20 C19 116.3(3) . . ?
C21 C20 C19 122.7(4) . . ?
C22 C21 C20 119.2(4) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C23 C22 C21 119.8(5) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 118.0(5) . . ?
C22 C23 H23 121.0 . . ?
C24 C23 H23 121.0 . . ?
N8 C24 C23 123.2(5) . . ?
N8 C24 H24 118.4 . . ?
C23 C24 H24 118.4 . . ?
N9 C25 N10 171.1(5) . . ?
N11 C26 N10 173.5(6) . . ?
Mn1 O1 H1A 118(2) . . ?
Mn1 O1 H1B 132(2) . . ?
H1A O1 H1B 109(2) . . ?
H2A O2 H2B 117(3) . . ?
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
Cr1 C2 2.063(4) . ?
Cr1 C4 2.066(4) . ?
Cr1 C3 2.066(4) . ?
Cr1 N6 2.073(3) . ?
Cr1 N5 2.079(3) . ?
Cr1 C1 2.086(4) . ?
Mn1 N9 2.171(4) . ?
Mn1 O1 2.219(3) . ?
Mn1 N1 2.226(3) 1_545 ?
Mn1 N7 2.233(3) . ?
Mn1 N2 2.246(3) . ?
Mn1 N8 2.255(3) . ?
N1 C1 1.143(4) . ?
N1 Mn1 2.226(3) 1_565 ?
N2 C2 1.134(4) . ?
N3 C3 1.142(4) . ?
N4 C4 1.146(4) . ?
N5 C5 1.342(4) . ?
N5 C9 1.363(4) . ?
N6 C10 1.351(4) . ?
N6 C14 1.353(4) . ?
N7 C15 1.341(4) . ?
N7 C19 1.352(4) . ?
N8 C24 1.332(5) . ?
N8 C20 1.339(4) . ?
N9 C25 1.127(5) . ?
N10 C25 1.273(6) . ?
N10 C26 1.285(6) . ?
N11 C26 1.130(6) . ?
C5 C6 1.378(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.373(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.377(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.470(5) . ?
C10 C11 1.393(5) . ?
C11 C12 1.379(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.364(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.382(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.372(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.369(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.365(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.375(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.485(5) . ?
C20 C21 1.392(5) . ?
C21 C22 1.377(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.357(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.385(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
O1 H1A 0.930(17) . ?
O1 H1B 0.932(17) . ?
O2 H2A 0.903(17) . ?
O2 H2B 0.890(17) . ?
