#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:47:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179128 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/90/4309054.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_4309054
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            'C15 H18 Cr Mn N9 O4'
_chemical_formula_weight         495.32
_chemical_name_common            Cr(bpy)Mn-N3
_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                102.0137(11)
_cell_angle_beta                 92.9851(12)
_cell_angle_gamma                111.6520(11)
_cell_formula_units_Z            2
_cell_length_a                   8.3864(3)
_cell_length_b                   10.8986(3)
_cell_length_c                   12.9321(4)
_cell_measurement_reflns_used    11325
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     1063.68(6)
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23143
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4870
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0387P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                2589
_reflns_number_total             4870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0484194si20041117_040813_6.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4309054
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.44274(6) 0.78679(4) 0.20731(4) 0.03016(14) Uani 1 1 d . . .
Cr1 Cr 0.43583(6) 0.28553(4) 0.20111(4) 0.02507(14) Uani 1 1 d . . .
O1 O 0.1557(3) 0.7009(3) 0.1899(3) 0.0663(8) Uani 1 1 d . . .
O2 O 0.4153(4) 0.8138(2) 0.3809(2) 0.0581(7) Uani 1 1 d D . .
O3 O 0.1862(4) 0.5818(3) 0.4299(2) 0.0689(8) Uani 1 1 d D . .
O4 O 0.2709(4) 0.9883(3) 0.4721(3) 0.1010(11) Uani 1 1 d D . .
N1 N 0.8174(4) 0.4141(3) 0.3342(3) 0.0553(8) Uani 1 1 d . . .
N2 N 0.5578(4) 0.2580(3) -0.0304(2) 0.0415(7) Uani 1 1 d . . .
N3 N 0.4305(3) -0.0113(2) 0.2060(2) 0.0356(7) Uani 1 1 d . . .
N4 N 0.4406(4) 0.5831(3) 0.2062(2) 0.0402(7) Uani 1 1 d . . .
N5 N 0.1797(3) 0.2113(2) 0.13245(19) 0.0277(6) Uani 1 1 d . . .
N6 N 0.3110(3) 0.2825(2) 0.33502(19) 0.0283(6) Uani 1 1 d . . .
N7 N 0.7199(4) 0.8794(3) 0.2495(3) 0.0735(12) Uani 1 1 d . . .
N8 N 0.8506(4) 0.8699(3) 0.2636(2) 0.0487(8) Uani 1 1 d . . .
N9 N 0.9878(5) 0.8690(4) 0.2789(3) 0.0901(13) Uani 1 1 d . . .
C1 C 0.6826(5) 0.3688(3) 0.2849(3) 0.0358(8) Uani 1 1 d . . .
C2 C 0.5240(4) 0.2720(3) 0.0543(3) 0.0318(7) Uani 1 1 d . . .
C3 C 0.4288(4) 0.0920(3) 0.2023(2) 0.0277(7) Uani 1 1 d . . .
C4 C 0.4444(4) 0.4789(3) 0.2037(2) 0.0306(7) Uani 1 1 d . . .
C5 C 0.1220(4) 0.1851(3) 0.0288(3) 0.0367(8) Uani 1 1 d . . .
H5 H 0.2021 0.1985 -0.0191 0.044 Uiso 1 1 calc R . .
C6 C -0.0510(4) 0.1390(3) -0.0100(3) 0.0434(9) Uani 1 1 d . . .
H6 H -0.0866 0.1229 -0.0826 0.052 Uiso 1 1 calc R . .
C7 C -0.1697(4) 0.1174(3) 0.0595(3) 0.0432(9) Uani 1 1 d . . .
H7 H -0.2874 0.0844 0.0347 0.052 Uiso 1 1 calc R . .
C8 C -0.1134(4) 0.1447(3) 0.1656(3) 0.0383(8) Uani 1 1 d . . .
H8 H -0.1929 0.1313 0.2139 0.046 Uiso 1 1 calc R . .
C9 C 0.0621(4) 0.1924(3) 0.2016(3) 0.0314(7) Uani 1 1 d . . .
C10 C 0.1362(4) 0.2292(3) 0.3149(3) 0.0314(7) Uani 1 1 d . . .
C11 C 0.0364(5) 0.2151(3) 0.3975(3) 0.0452(9) Uani 1 1 d . . .
H11 H -0.0839 0.1773 0.3826 0.054 Uiso 1 1 calc R . .
C12 C 0.1166(5) 0.2574(4) 0.5009(3) 0.0519(10) Uani 1 1 d . . .
H12 H 0.0511 0.2496 0.5568 0.062 Uiso 1 1 calc R . .
C13 C 0.2938(5) 0.3114(3) 0.5213(3) 0.0484(9) Uani 1 1 d . . .
H13 H 0.3501 0.3406 0.5912 0.058 Uiso 1 1 calc R . .
C14 C 0.3877(5) 0.3218(3) 0.4368(3) 0.0399(8) Uani 1 1 d . . .
H14 H 0.5080 0.3571 0.4507 0.048 Uiso 1 1 calc R . .
C15 C 0.0400(7) 0.5758(6) 0.1363(5) 0.144(3) Uani 1 1 d . . .
H15A H 0.0056 0.5780 0.0650 0.216 Uiso 1 1 calc R . .
H15B H -0.0601 0.5503 0.1724 0.216 Uiso 1 1 calc R . .
H15C H 0.0924 0.5106 0.1337 0.216 Uiso 1 1 calc R . .
H3W H 0.0599 0.5498 0.4038 0.29(4) Uiso 1 1 d RD . .
H4W H 0.1383 0.5802 0.4982 0.22(3) Uiso 1 1 d RD . .
H1W H 0.3009 0.7982 0.3486 0.16(3) Uiso 1 1 d RD . .
H2W H 0.3321 0.7360 0.4139 0.18(3) Uiso 1 1 d RD . .
H1 H 0.1307 0.8063 0.1982 0.42(6) Uiso 1 1 d R . .
H5W H 0.3610 0.9347 0.4296 0.076(12) Uiso 1 1 d RD . .
H6W H 0.3408 1.0807 0.5327 1.2(3) Uiso 1 1 d RD . .
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'
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'
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
N7 Mn1 N4 91.49(11) . . ?
N7 Mn1 O1 171.39(14) . . ?
N4 Mn1 O1 89.56(10) . . ?
N7 Mn1 N2 96.17(13) . 2_665 ?
N4 Mn1 N2 89.43(10) . 2_665 ?
O1 Mn1 N2 92.39(11) . 2_665 ?
N7 Mn1 O2 89.41(14) . . ?
N4 Mn1 O2 88.00(9) . . ?
O1 Mn1 O2 82.09(11) . . ?
N2 Mn1 O2 173.92(10) 2_665 . ?
N7 Mn1 N3 91.38(11) . 1_565 ?
N4 Mn1 N3 177.12(10) . 1_565 ?
O1 Mn1 N3 87.61(10) . 1_565 ?
N2 Mn1 N3 90.20(9) 2_665 1_565 ?
O2 Mn1 N3 92.10(10) . 1_565 ?
C1 Cr1 N5 173.59(11) . . ?
C1 Cr1 N6 95.27(11) . . ?
N5 Cr1 N6 78.82(10) . . ?
C1 Cr1 C2 93.24(13) . . ?
N5 Cr1 C2 92.74(11) . . ?
N6 Cr1 C2 171.41(11) . . ?
C1 Cr1 C4 90.34(12) . . ?
N5 Cr1 C4 87.27(10) . . ?
N6 Cr1 C4 90.49(11) . . ?
C2 Cr1 C4 90.70(11) . . ?
C1 Cr1 C3 88.85(11) . . ?
N5 Cr1 C3 93.43(10) . . ?
N6 Cr1 C3 88.53(10) . . ?
C2 Cr1 C3 90.41(11) . . ?
C4 Cr1 C3 178.66(12) . . ?
C15 O1 Mn1 129.8(3) . . ?
C2 N2 Mn1 166.6(3) . 2_665 ?
C3 N3 Mn1 177.2(3) . 1_545 ?
C4 N4 Mn1 177.6(3) . . ?
C5 N5 C9 118.2(3) . . ?
C5 N5 Cr1 126.4(2) . . ?
C9 N5 Cr1 115.4(2) . . ?
C14 N6 C10 118.8(3) . . ?
C14 N6 Cr1 126.0(2) . . ?
C10 N6 Cr1 115.1(2) . . ?
N8 N7 Mn1 150.3(3) . . ?
N7 N8 N9 175.7(4) . . ?
N1 C1 Cr1 177.9(3) . . ?
N2 C2 Cr1 174.0(3) . . ?
N3 C3 Cr1 177.4(3) . . ?
N4 C4 Cr1 176.5(3) . . ?
N5 C5 C6 122.7(3) . . ?
C7 C6 C5 119.1(3) . . ?
C8 C7 C6 119.1(3) . . ?
C7 C8 C9 120.0(3) . . ?
N5 C9 C8 120.9(3) . . ?
N5 C9 C10 115.0(3) . . ?
C8 C9 C10 124.1(3) . . ?
N6 C10 C11 121.0(3) . . ?
N6 C10 C9 115.5(3) . . ?
C11 C10 C9 123.5(3) . . ?
C12 C11 C10 119.5(3) . . ?
C11 C12 C13 119.5(3) . . ?
C12 C13 C14 119.0(3) . . ?
N6 C14 C13 122.2(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
Mn1 N7 2.151(3) . ?
Mn1 N4 2.210(3) . ?
Mn1 O1 2.217(3) . ?
Mn1 N2 2.238(3) 2_665 ?
Mn1 O2 2.238(3) . ?
Mn1 N3 2.244(3) 1_565 ?
Cr1 C1 2.062(4) . ?
Cr1 N5 2.068(2) . ?
Cr1 N6 2.070(2) . ?
Cr1 C2 2.070(3) . ?
Cr1 C4 2.075(3) . ?
Cr1 C3 2.091(3) . ?
O1 C15 1.357(5) . ?
N1 C1 1.145(4) . ?
N2 C2 1.139(4) . ?
N2 Mn1 2.238(3) 2_665 ?
N3 C3 1.142(3) . ?
N3 Mn1 2.244(3) 1_545 ?
N4 C4 1.143(3) . ?
N5 C5 1.335(4) . ?
N5 C9 1.354(4) . ?
N6 C14 1.343(4) . ?
N6 C10 1.350(4) . ?
N7 N8 1.147(4) . ?
N8 N9 1.161(4) . ?
C5 C6 1.375(4) . ?
C6 C7 1.364(5) . ?
C7 C8 1.361(4) . ?
C8 C9 1.384(4) . ?
C9 C10 1.473(4) . ?
C10 C11 1.390(4) . ?
C11 C12 1.369(5) . ?
C12 C13 1.369(5) . ?
C13 C14 1.380(4) . ?
