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_7023410
_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
'C74.5 H89 Co8 N16 O33, 3(Cl O4), 5(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C79.5 H113 Cl3 Co8 N16 O52'
_chemical_formula_weight         2702.65
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.2539(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.9059(4)
_cell_length_b                   14.9866(2)
_cell_length_c                   27.3422(4)
_cell_measurement_reflns_used    10240
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      29.2834
_cell_measurement_theta_min      2.6995
_cell_volume                     10612.8(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
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120.01(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  -20.00    7.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       13.9943  -94.0000  -81.0000 27

  2 omega  -37.00   46.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       13.9943  -57.0000  -90.0000 83

  3 omega    1.00   93.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       13.9943   37.0000   90.0000 92
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0014615000
_diffrn_orient_matrix_UB_12      0.0395864000
_diffrn_orient_matrix_UB_13      0.0141192000
_diffrn_orient_matrix_UB_21      -0.0168092000
_diffrn_orient_matrix_UB_22      0.0190954000
_diffrn_orient_matrix_UB_23      -0.0179508000
_diffrn_orient_matrix_UB_31      -0.0215750000
_diffrn_orient_matrix_UB_32      -0.0175612000
_diffrn_orient_matrix_UB_33      0.0123105000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20971
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91003
_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_colour_primary    orange
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5540
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.563
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         9391
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      5.185
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+97.1309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                8002
_reflns_number_total             9391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51301g.txt
_cod_data_source_block           merm
_cod_original_formula_sum        'C79.50 H113 Cl3 Co8 N16 O52'
_cod_database_code               7023410
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2H,H1H} of O2A, H14 of O16, H19A of O19, All C(H,H)
  groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H13A,H13B} of O13, H1B of O1B, H2B of O2B, {H2AA,
  H2AB} of O2A, H16 of O16
2. Shared sites
{O13, O19}
3. Restrained distances
 O1H-H1H
 0.84 with sigma of 0.02
 H2H-O2H
 0.84 with sigma of 0.02
 C13-H16
 2 with sigma of 0.02
 H14-O14
 0.84 with sigma of 0.02
 C1A-H19A
 2.1 with sigma of 0.02
 C1A-O19
 1.5 with sigma of 0.005
 Cl20-O22A = Cl20-O21A = Cl20-O15 = Cl20-O18
 1.44 with sigma of 0.005
 Cl10-O14A = Cl10-O12A = Cl10-O13A = Cl10-O11A = Cl10-O17 = Cl10-O1C = Cl10-O1D
 1.44 with sigma of 0.005
 O1D-O1C
 2.3 with sigma of 0.01
 O12A-O1C
 2.3 with sigma of 0.04
 O17-O1D
 2.3 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O13) = Uanis(O19)
Uanis(O17) = Uanis(O1C) = Uanis(O1D)
5. Others
 Fixed Sof: O13(0.75) H13A(0.75) H13B(0.75) O14A(0.7) Cl20(0.5) O13A(0.7)
 O11A(0.7) O15(0.5) O16(0.5) H16(0.5) O18(0.5) O19(0.25) H19A(0.25) C1A(0.25)
 H1AA(0.25) H1AB(0.25) H1AC(0.25) C1C(0.5) H1CA(0.5) H1CB(0.5) H1CC(0.5)
 O17(0.3) O1C(0.3) O1D(0.3)
6.a Free rotating group:
 O2A(H2H,H1H,H2AA,H2AB), O16(H14,H16)
6.b Rotating group:
 O13(H13A,H13B)
6.c Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C35(H35A,H35B), C16(H16A,H16B), C25(H25A,H25B), C34(H34A,
 H34B), C26(H26A,H26B), C8(H8A,H8B), C7(H7A,H7B)
6.d Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6), N8(H8), C11(H11), C1(H1), C28(H28), C13(H13), N2(H2),
 C31(H31), C30(H30), C12(H12), C10(H10), C19(H19), C21(H21), C29(H29), C2(H2A),
 C22(H22), C20(H20), C3(H3), C4(H4A)
6.e Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C1B(H1BA,H1BB,H1BC), C2B(H2BA,H2BB,H2BC), C1A(H1AA,H1AB,
 H1AC), C1C(H1CA,H1CB,H1CC)
6.f Idealised tetrahedral OH refined as rotating group:
 O1B(H1B), O2B(H2B)
;