#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:59:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179874 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/70/7017079.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_7017079
loop_
_publ_author_name
'Keene, Tony D.'
'Murphy, Michael J.'
'Price, Jason R.'
'Price, David J.'
'Kepert, Cameron J.'
_publ_section_title
;
 A new modification of an old framework: Hofmann layers with unusual
 tetracyanidometallate groups.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11621
_journal_page_last               11628
_journal_paper_doi               10.1039/c1dt11183c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C22 H14 Mn Mo N7 O2, 2(C0.50 H2 O0.50)'
_chemical_formula_sum            'C23 H18 Mn Mo N7 O3'
_chemical_formula_weight         591.32
_chemical_melting_point          ?
_chemical_name_common            'MoMn(bpa) Hofmann'
_chemical_name_systematic
;
{[Mn(H₂O)₂]~0.5~[Mn(bpa)₂]~0.5~
[Mo(O)(CN)₄(bpa)~0.5~]}.MeOH
;
_space_group_IT_number           10
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 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                 106.545(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2987(7)
_cell_length_b                   7.6559(3)
_cell_length_c                   14.6269(6)
_cell_measurement_reflns_used    5412
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.2499
_cell_measurement_theta_min      2.8997
_cell_volume                     1320.21(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Diamond 3.2g (Crystal Impact, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 10.5861
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11530
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.010
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1231P)²+5.9471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.2038
_reflns_number_gt                2104
_reflns_number_total             2515
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c1dt11183c.txt
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'N/A' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               7017079
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'-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
Mo1 Mo -0.09884(6) 0.5000 0.23261(4) 0.0245(3) Uani 1 2 d S . .
Mn1 Mn 0.0000 1.0000 0.0000 0.0243(5) Uani 1 4 d S . .
O1W O 0.1890(6) 1.0000 0.0470(5) 0.0456(18) Uani 1 2 d S . .
H1W1 H 0.2170 1.0295 -0.0060 0.068 Uiso 0.25 1 calc PR . .
H1W2 H 0.2159 0.8861 0.0703 0.068 Uiso 0.50 1 calc PR . .
H1W3 H 0.2155 1.0844 0.0969 0.068 Uiso 0.25 1 calc PR . .
N2 N -0.0107(5) 0.7961(7) 0.1051(4) 0.0345(13) Uani 1 1 d . . .
O1 O -0.2372(6) 0.5000 0.1748(5) 0.0445(17) Uani 1 2 d S . .
N11 N 0.1020(6) 0.5000 0.3238(5) 0.0300(17) Uani 1 2 d S . .
C16 C 0.4502(9) 0.5000 0.4781(8) 0.048(3) Uani 1 2 d S . .
N1 N -0.0881(5) 0.2033(7) 0.3981(4) 0.0318(12) Uani 1 1 d . . .
C2 C -0.0377(5) 0.6940(9) 0.1518(4) 0.0299(14) Uani 1 1 d . . .
C13 C 0.2488(9) 0.5000 0.4719(7) 0.049(3) Uani 1 2 d S . .
H13 H 0.2679 0.5000 0.5382 0.059 Uiso 1 2 calc SR . .
C11 C 0.1370(8) 0.5000 0.4202(6) 0.041(2) Uani 1 2 d S . .
H11 H 0.0824 0.5000 0.4530 0.050 Uiso 1 2 calc SR . .
C12 C 0.1856(9) 0.5000 0.2811(8) 0.046(3) Uani 1 2 d S . .
H12 H 0.1643 0.5000 0.2148 0.055 Uiso 1 2 calc SR . .
C1 C -0.0963(5) 0.3053(8) 0.3388(4) 0.0256(13) Uani 1 1 d . . .
C15 C 0.3336(8) 0.5000 0.4275(7) 0.042(2) Uani 1 2 d S . .
Mn2 Mn 0.0000 0.0000 0.5000 0.0246(5) Uani 1 4 d S . .
N21 N 0.1438(7) 0.0000 0.4311(5) 0.0316(17) Uani 1 2 d S . .
C14 C 0.2973(9) 0.5000 0.3266(8) 0.047(3) Uani 1 2 d S . .
H14 H 0.3502 0.5000 0.2921 0.056 Uiso 1 2 calc SR . .
N22 N 0.7031(10) 0.0506(14) 0.0899(8) 0.044(3) Uiso 0.50 1 d P A -1
C30 C 0.534(2) 0.145(3) 0.1308(18) 0.098(7) Uiso 0.50 1 d P A -1
H30 H 0.4682 0.2123 0.1147 0.118 Uiso 0.50 1 calc PR A -1
C32 C 0.613(2) 0.138(4) 0.073(2) 0.111(9) Uiso 0.50 1 d P A -1
H32 H 0.5947 0.2058 0.0180 0.134 Uiso 0.50 1 calc PR A -1
C28 C 0.5645(11) 0.0457(15) 0.2086(9) 0.038(3) Uiso 0.50 1 d P A -1
C24 C 0.3402(10) 0.0437(14) 0.4470(9) 0.034(3) Uiso 0.50 1 d P A -1
H24 H 0.4131 0.0599 0.4872 0.040 Uiso 0.50 1 calc PR A -1
C22 C 0.2495(9) 0.0381(14) 0.4845(8) 0.030(3) Uiso 0.50 1 d P A -1
H22 H 0.2617 0.0616 0.5490 0.036 Uiso 0.50 1 calc PR A -1
C23 C 0.2136(8) -0.0333(15) 0.2948(7) 0.027(3) Uiso 0.50 1 d P A -1
H23 H 0.2015 -0.0737 0.2327 0.033 Uiso 0.50 1 calc PR A -1
C21 C 0.1267(8) -0.0276(18) 0.3368(7) 0.026(3) Uiso 0.50 1 d P A -1
H21 H 0.0528 -0.0434 0.2985 0.032 Uiso 0.50 1 calc PR A -1
C26 C 0.4156(9) 0.0345(17) 0.3082(8) 0.033(3) Uiso 0.50 1 d P A -1
C27 C 0.4878(10) 0.0389(16) 0.2670(9) 0.037(3) Uiso 0.50 1 d P A -1
C25 C 0.3237(8) 0.025(2) 0.3502(7) 0.029(3) Uiso 0.50 1 d P A -1
C29 C 0.6680(12) -0.038(2) 0.2304(11) 0.053(4) Uiso 0.50 1 d P A -1
H29 H 0.6937 -0.0989 0.2877 0.064 Uiso 0.50 1 calc PR A -1
C31 C 0.7330(10) -0.0336(19) 0.1686(8) 0.053(4) Uiso 0.50 1 d P A -1
H31 H 0.8015 -0.0938 0.1844 0.063 Uiso 0.50 1 calc PR A -1
O91 O 0.2868(10) 0.6614(19) 0.1056(8) 0.140(7) Uiso 0.50 1 d PR A -2
H91 H 0.2461 0.7428 0.0799 0.210 Uiso 0.50 1 calc PR A -2
C92 C 0.240(2) 0.5000 0.0613(19) 0.144(9) Uiso 0.5 2 d S A -2
H92A H 0.2788 0.4037 0.0986 0.216 Uiso 0.50 1 calc PR A -2
H92B H 0.2488 0.4939 -0.0017 0.216 Uiso 0.50 1 calc SR A -2
H92C H 0.1607 0.4946 0.0575 0.216 Uiso 0.50 1 calc SR A -2
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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
O1 Mo1 C1 99.7(2) . 4_565
O1 Mo1 C1 99.7(2) . .
C1 Mo1 C1 88.0(3) 4_565 .
O1 Mo1 C2 100.7(2) . .
C1 Mo1 C2 89.0(2) 4_565 .
C1 Mo1 C2 159.5(2) . .
O1 Mo1 C2 100.7(2) . 4_565
C1 Mo1 C2 159.5(2) 4_565 4_565
C1 Mo1 C2 89.0(2) . 4_565
C2 Mo1 C2 86.8(3) . 4_565
O1 Mo1 N11 177.6(3) . .
C1 Mo1 N11 78.5(2) 4_565 .
C1 Mo1 N11 78.5(2) . .
C2 Mo1 N11 81.0(2) . .
C2 Mo1 N11 81.0(2) 4_565 .
N2 Mn1 N2 180.00(19) 2 4_575
N2 Mn1 N2 90.7(3) 2 .
N2 Mn1 N2 89.3(3) 4_575 .
N2 Mn1 N2 89.3(3) 2 3_575
N2 Mn1 N2 90.7(3) 4_575 3_575
N2 Mn1 N2 180.0(3) . 3_575
N2 Mn1 O1W 87.20(19) 2 .
N2 Mn1 O1W 92.80(19) 4_575 .
N2 Mn1 O1W 92.80(19) . .
N2 Mn1 O1W 87.20(19) 3_575 .
N2 Mn1 O1W 92.80(19) 2 3_575
N2 Mn1 O1W 87.20(19) 4_575 3_575
N2 Mn1 O1W 87.20(19) . 3_575
N2 Mn1 O1W 92.80(19) 3_575 3_575
O1W Mn1 O1W 180.0 . 3_575
Mn1 O1W H1W1 109.5 . .
Mn1 O1W H1W2 109.5 . .
H1W1 O1W H1W2 109.5 . .
Mn1 O1W H1W3 109.5 . .
H1W1 O1W H1W3 109.5 . .
H1W2 O1W H1W3 109.5 . .
C2 N2 Mn1 167.1(5) . .
C12 N11 C11 115.2(8) . .
C12 N11 Mo1 122.1(6) . .
C11 N11 Mo1 122.7(6) . .
C16 C16 C15 179.6(16) 3_666 .
C1 N1 Mn2 155.0(5) . .
N2 C2 Mo1 176.3(6) . .
C11 C13 C15 121.1(9) . .
C11 C13 H13 119.5 . .
C15 C13 H13 119.5 . .
N11 C11 C13 123.2(9) . .
N11 C11 H11 118.4 . .
C13 C11 H11 118.4 . .
N11 C12 C14 125.3(10) . .
N11 C12 H12 117.3 . .
C14 C12 H12 117.3 . .
N1 C1 Mo1 175.9(5) . .
C13 C15 C14 115.9(9) . .
C13 C15 C16 122.9(10) . .
C14 C15 C16 121.2(10) . .
N1 Mn2 N1 180.0(2) 4 2_556
N1 Mn2 N1 89.4(3) 4 .
N1 Mn2 N1 90.6(3) 2_556 .
N1 Mn2 N1 90.6(3) 4 3_556
N1 Mn2 N1 89.4(3) 2_556 3_556
N1 Mn2 N1 180.000(1) . 3_556
N1 Mn2 N21 90.28(19) 4 3_556
N1 Mn2 N21 89.72(19) 2_556 3_556
N1 Mn2 N21 90.28(19) . 3_556
N1 Mn2 N21 89.72(19) 3_556 3_556
N1 Mn2 N21 89.72(19) 4 .
N1 Mn2 N21 90.28(19) 2_556 .
N1 Mn2 N21 89.72(19) . .
N1 Mn2 N21 90.28(19) 3_556 .
N21 Mn2 N21 180.000(1) 3_556 .
C22 N21 C22 25.1(10) . 4
C22 N21 C21 113.8(8) . 4
C22 N21 C21 118.1(8) 4 4
C22 N21 C21 118.1(8) . .
C22 N21 C21 113.8(8) 4 .
C21 N21 C21 18.0(12) 4 .
C22 N21 Mn2 119.2(6) . .
C22 N21 Mn2 119.2(6) 4 .
C21 N21 Mn2 122.6(6) 4 .
C21 N21 Mn2 122.6(6) . .
C12 C14 C15 119.4(9) . .
C12 C14 H14 120.3 . .
C15 C14 H14 120.3 . .
C32 N22 C31 117.0(18) . .
C28 C30 C32 114(2) . .
C28 C30 H30 123.2 . .
C32 C30 H30 123.2 . .
N22 C32 C30 127(3) . .
N22 C32 H32 116.5 . .
C30 C32 H32 116.5 . .
C30 C28 C29 118.8(16) . .
C30 C28 C27 116.9(16) . .
C29 C28 C27 124.2(12) . .
C22 C24 C25 120.4(11) . .
C22 C24 H24 119.8 . .
C25 C24 H24 119.8 . .
N21 C22 C24 122.3(10) . .
N21 C22 H22 118.9 . .
C24 C22 H22 118.9 . .
C21 C23 C25 117.7(9) . .
C21 C23 H23 121.1 . .
C25 C23 H23 121.1 . .
N21 C21 C23 123.0(9) . .
N21 C21 H21 118.5 . .
C23 C21 H21 118.5 . .
C27 C26 C25 175.5(12) . .
C26 C27 C28 174.0(13) . .
C24 C25 C26 122.1(10) . .
C24 C25 C23 116.7(10) . .
C26 C25 C23 120.3(10) . .
C31 C29 C28 120.6(14) . .
C31 C29 H29 119.7 . .
C28 C29 H29 119.7 . .
N22 C31 C29 122.5(13) . .
N22 C31 H31 118.7 . .
C29 C31 H31 118.7 . .
C92 O91 H91 109.5 . .
O91 C92 H92A 109.5 . .
O91 C92 H92B 109.5 . .
H92A C92 H92B 109.5 . .
O91 C92 H92C 109.5 . .
H92A C92 H92C 109.5 . .
H92B C92 H92C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.670(7) .
Mo1 C1 2.147(6) 4_565
Mo1 C1 2.147(6) .
Mo1 C2 2.162(6) .
Mo1 C2 2.162(6) 4_565
Mo1 N11 2.451(7) .
Mn1 N2 2.221(5) 2
Mn1 N2 2.221(5) 4_575
Mn1 N2 2.221(5) .
Mn1 N2 2.221(5) 3_575
Mn1 O1W 2.228(7) .
Mn1 O1W 2.228(7) 3_575
O1W H1W1 0.9600 .
O1W H1W2 0.9600 .
O1W H1W3 0.9600 .
N2 C2 1.147(8) .
N11 C12 1.345(12) .
N11 C11 1.353(11) .
C16 C16 1.21(2) 3_666
C16 C15 1.414(14) .
N1 C1 1.150(8) .
N1 Mn2 2.213(5) .
C13 C11 1.367(14) .
C13 C15 1.378(14) .
C13 H13 0.9300 .
C11 H11 0.9300 .
C12 C14 1.346(15) .
C12 H12 0.9300 .
C15 C14 1.414(15) .
Mn2 N1 2.213(5) 4
Mn2 N1 2.213(5) 2_556
Mn2 N1 2.213(5) 3_556
Mn2 N21 2.272(7) 3_556
Mn2 N21 2.272(7) .
N21 C22 1.344(13) .
N21 C22 1.344(13) 4
N21 C21 1.351(12) 4
N21 C21 1.351(12) .
C14 H14 0.9300 .
N22 C32 1.26(3) .
N22 C31 1.279(16) .
C30 C28 1.33(3) .
C30 C32 1.46(3) .
C30 H30 0.9300 .
C32 H32 0.9300 .
C28 C29 1.380(18) .
C28 C27 1.443(17) .
C24 C22 1.377(16) .
C24 C25 1.379(16) .
C24 H24 0.9300 .
C22 H22 0.9300 .
C23 C21 1.376(14) .
C23 C25 1.438(15) .
C23 H23 0.9300 .
C21 H21 0.9300 .
C26 C27 1.207(16) .
C26 C25 1.433(14) .
C29 C31 1.368(18) .
C29 H29 0.9300 .
C31 H31 0.9300 .
O91 C92 1.437(18) .
O91 H91 0.8200 .
C92 H92A 0.9600 .
C92 H92B 0.9600 .
C92 H92C 0.9600 .
