Synthesis, structural and magnetic characterisation of iron(II/III), cobalt(II) and copper(II) cluster complexes of the polytopic ligand: N-(2-pyridyl)-3-carboxypropanamide.
Russell, Mark E.; Hawes, Chris S.; Ferguson, Alan; Polson, Matthew I. J.; Chilton, Nicholas F.; Moubaraki, Boujemaa; Murray, Keith S.; Kruger, Paul E.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 13576–13583; doi:10.1039/c3dt51301g

data_7023409
_publ_section_title
;
 Synthesis, structural and magnetic characterisation of iron(II/III),
 cobalt(II) and copper(II) cluster complexes of the polytopic ligand:
 N-(2-pyridyl)-3-carboxypropanamide.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13576
_journal_page_last               13583
_journal_paper_doi               10.1039/c3dt51301g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety
'C54 H60 Fe5 N12 O22, 5(Cl O4), 3(C2 H3 N), 4(H2 O)'
_chemical_formula_sum            'C60 H77 Cl5 Fe5 N15 O46'
_chemical_formula_weight         2200.82
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-14
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.0441(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2556(2)
_cell_length_b                   22.8571(4)
_cell_length_c                   25.5874(4)
_cell_measurement_reflns_used    16167
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      73.6676
_cell_measurement_theta_min      2.7772
_cell_volume                     9297.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120.02(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -49.00   36.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063   37.0000  150.0000 85
 
  2 omega -114.00  -10.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063  -57.0000    0.0000 104
 
  3 omega   66.00   96.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       39.9063 -125.0000   90.0000 30
 
  4 omega   35.00   62.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       39.9063 -125.0000 -150.0000 27
 
  5 omega   32.00   88.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000 -120.0000 56
 
  6 omega   52.00   91.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -35.0000  -79.0000 39
 
  7 omega   85.00  141.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   45.0000   90.0000 56
 
  8 omega   57.00   93.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000  -30.0000 36
 
  9 omega   37.00  105.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000 -150.0000 68
 
 10 omega   42.00   80.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  120.0000 38
 
 11 omega   33.00   99.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -180.0000 66
 
 12 omega   79.00  169.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000 -180.0000 90
 
 13 omega -119.00   -6.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063  -77.0000 -180.0000 113
 
 14 omega -114.00  -10.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063  -57.0000 -120.0000 104
 
 15 omega  -49.00   36.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063   37.0000  -60.0000 85
 
 16 omega   77.00  168.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000    0.0000 91
 
 17 omega   77.00  178.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   61.0000  -90.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0042662000
_diffrn_orient_matrix_UB_12      -0.0302261000
_diffrn_orient_matrix_UB_13      0.0531886000
_diffrn_orient_matrix_UB_21      0.0968281000
_diffrn_orient_matrix_UB_22      -0.0005435000
_diffrn_orient_matrix_UB_23      0.0155422000
_diffrn_orient_matrix_UB_31      -0.0012794000
_diffrn_orient_matrix_UB_32      0.0602070000
_diffrn_orient_matrix_UB_33      0.0268362000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            56674
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4364
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         1.402
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1199
_refine_ls_number_reflns         16567
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.1325
_refine_ls_R_factor_gt           0.0998
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3016
_refine_ls_wR_factor_ref         0.3250
_reflns_number_gt                10965
_reflns_number_total             16567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51301g.txt
_cod_data_source_block           mer27squeeze-sr
_cod_original_cell_volume        9297.9(2)
_cod_database_code               7023409
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O26-O27 = O26-O28 = O26-O29 = O27-O28 = O27-O29 = O28-O29
 2.29 with sigma of 0.02
 N15-C60
 1.15 with sigma of 0.02
 N25-C62
 1.15 with sigma of 0.02
 N19-C58
 1.15 with sigma of 0.02
 O46-O47 = O46-O48 = O46-O49 = O47-O48 = O47-O49 = O48-O49
 2.29 with sigma of 0.02
 C63-C62
 1.45 with sigma of 0.02
 C60-C61
 1.45 with sigma of 0.02
 C58-C59
 1.45 with sigma of 0.02
 H2BA-H64A
 2 with sigma of 0.02
 C28-C29
 1.39 with sigma of 0.02
 C29-C30
 1.39 with sigma of 0.02
 C30-C31
 1.39 with sigma of 0.02
 N7-C28
 1.39 with sigma of 0.02
 N7-C32
 1.39 with sigma of 0.02
 C32-C1B
 1.39 with sigma of 0.02
 C1B-C1A
 1.39 with sigma of 0.02
 C1A-C1D
 1.39 with sigma of 0.02
 C1D-C28
 1.39 with sigma of 0.02
 C31-C1C
 1.39 with sigma of 0.02
 C1C-N7
 1.39 with sigma of 0.02
 Cl10-O56 = Cl10-O53 = Cl10-O1F = Cl10-O1J
 1.44 with sigma of 0.02
 Cl4-O37 = Cl4-O35 = Cl4-O31 = Cl4-O32 = Cl4-O33 = Cl4-O30 = Cl4-O34 = Cl4-O36
 1.44 with sigma of 0.02
 Cl7-O46 = Cl7-O47 = Cl7-O48 = Cl7-O49
 1.44 with sigma of 0.02
 Cl7-O48 = Cl7-O46 = Cl7-O49 = Cl7-O47
 1.44 with sigma of 0.02
 Cl3-O26 = Cl3-O27 = Cl3-O28 = Cl3-O29
 1.44 with sigma of 0.02
 Cl3-O26 = Cl3-O27 = Cl3-O29 = Cl3-O28
 1.44 with sigma of 0.02
 Cl2-O22 = Cl2-O23 = Cl2-O20 = Cl2-O21
 1.44 with sigma of 0.02
 Cl1-O22 = Cl1-O23 = Cl1-O24 = Cl1-O25
 1.44 with sigma of 0.02
 Cl9-O1D
 1.44 with sigma of 0.02
 Cl9-O24
 1.44 with sigma of 0.02
 Cl9-O22 = Cl9-O1C
 1.44 with sigma of 0.02
 Cl6-O45 = Cl6-O42 = Cl6-O44 = Cl6-O43
 1.44 with sigma of 0.02
 Cl8-O54 = Cl8-O55 = Cl8-O1H = Cl8-O1I
 1.44 with sigma of 0.02
 Cl5-O41 = Cl5-O39 = Cl5-O38 = Cl5-O40
 1.44 with sigma of 0.02
 O22-O1C
 2.3 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C30 \\sim C29: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.
Cl1 \\sim O24 \\sim O22 \\sim O25 \\sim O23: within 1.7A with sigma of 0.04 and
Cl6 \\sim O45 \\sim O44 \\sim O42 \\sim O43: within 1.7A with sigma of 0.04 and
Uanis(O34) = Uanis(O35)
Uanis(O31) = Uanis(O30)
Uanis(O32) = Uanis(O33)
Uanis(O36) = Uanis(O37)
Uiso(N25) = Uiso(C62) = Uiso(C63)
Uanis(N14) = Uanis(C1C)
Uanis(Cl10) = Uanis(O1F) = Uanis(O53) = Uanis(O56) = Uanis(O1J)
Uiso(O48) = Uiso(Cl7) = Uiso(O47) = Uiso(O49) = Uiso(O46)
Uiso(O27) = Uiso(O26) = Uiso(O28) = Uiso(Cl3) = Uiso(O29)
Uanis(Cl1) = Uanis(O22) = Uanis(O24) = Uanis(O25) = Uanis(Cl2) = Uanis(Cl9) = Ua
Uanis(O45) = Uanis(Cl6) = Uanis(O44) = Uanis(O42) = Uanis(O43)
Uanis(Cl8) = Uanis(O1I) = Uanis(O1H) = Uanis(O54) = Uanis(O55)
4. Others
 Fixed Sof: O37(0.25) N8(0.6) H8(0.6) O35(0.75) O31(0.75) C32(0.6) O54(0.5)
 H28A(0.5) H28(0.5) O55(0.5) C31(0.4) H31(0.4) Cl5(0.5) O41(0.5) O39(0.5)
 O38(0.5) O40(0.5) Cl1(0.4) O23(0.8) O24(0.6) Cl6(0.5) O45(0.5) Cl2(0.4)
 N13(0.5) C65(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) N15(0.5) C60(0.5)
 C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) N19(0.5) C58(0.5) C59(0.5) H59A(0.5)
 H59B(0.5) H59C(0.5) O25(0.4) O20(0.4) O21(0.4) C29(0.4) H29(0.4) C30(0.4)
 H30(0.4) O32(0.75) O42(0.5) O56(0.5) Cl8(0.5) O33(0.25) O30(0.25) O34(0.25)
 O36(0.75) O53(0.5) O50(0.5) Cl3(0.5) O48(0.5) Cl7(0.5) O46(0.5) O26(0.5)
 O49(0.5) O27(0.5) O29(0.5) O44(0.5) O43(0.5) O47(0.5) N25(0.5) C62(0.5)
 C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) O28(0.5) C1A(0.6) H1A(0.6) C1B(0.6)
 H1B(0.6) C1C(0.4) C1D(0.6) H1D(0.6) N14(0.4) H14(0.4) Cl9(0.2) O1C(0.2)
 O1D(0.2) O1E(0.5) H1EA(0.5) H1EB(0.5) O1F(0.5) Cl10(0.5) O1H(0.5) O1I(0.5)
 O1J(0.5)
 Fixed Uiso: Cl3(0.12) O48(0.12) Cl7(0.12) O46(0.12) O26(0.12) O49(0.12)
 O27(0.12) O29(0.12) O47(0.12) O28(0.12)
5.a Riding coordinates:
 N14(H14)
5.b Free rotating group:
 O52(H52C,H52D), O51(H51A,H51B), O1E(H1EA,H1EB)
5.c Rotating group:
 O1B(H1BA,H1BB), O3B(H3BA,H3BB), O2B(H2BA,H2BB)
5.d Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C17(H17A,H17B), C8(H8A,H8B), C7(H7A,H7B), C44(H44A,H44B),
 C43(H43A,H43B), C16(H16A,H16B), C52(H52A,H52B), C53(H53A,H53B), C25(H25A,H25B),
  C34(H34A,H34B), C35(H35A,H35B)
5.e Aromatic/amide H refined with riding coordinates:
 N10(H10), N6(H6), N4(H4), N2(H2), N12(H12), N8(H8), C40(H40), C19(H19),
 C21(H21), C1(H1), C22(H22), C38(H38), C37(H37), C2(H2A), C4(H4A), C20(H20),
 C49(H49), C39(H39), C13(H13), C3(H3), C48(H48), C12(H12A), C46(H46), C11(H11),
 C10(H10A), C28(H28A), C28(H28), C47(H47), C31(H31), C29(H29), C30(H30),
 C1A(H1A), C1B(H1B), C1D(H1D)
5.f Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C61(H61A,H61B,H61C), C59(H59A,H59B,H59C), C63(H63A,H63B,
 H63C)
;