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_7023411
_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         'C37 H38 Cu6 N8 O20, C H4 O'
_chemical_formula_sum            'C38 H42 Cu6 N8 O21'
_chemical_formula_weight         1328.04
_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                 91.5503(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   41.7229(8)
_cell_length_b                   13.7165(3)
_cell_length_c                   15.3592(3)
_cell_measurement_reflns_used    8118
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.7720
_cell_measurement_theta_min      2.8757
_cell_volume                     8786.7(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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega   14.00   39.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063   77.0000  120.0000 25

  2 omega -116.00   -9.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063  -72.0000  118.0000 107

  3 omega  -71.00  -45.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063   77.0000  120.0000 26

  4 omega  -65.00   21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.9063   57.0000  -90.0000 86

  5 omega  126.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000  -60.0000 51

  6 omega   40.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000  120.0000 59

  7 omega  105.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   45.0000 -180.0000 71

  8 omega  152.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000    0.0000 26

  9 omega   39.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000    0.0000 52

 10 omega   98.00  124.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000    0.0000 26

 11 omega   37.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000 -150.0000 52

 12 omega  100.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000  120.0000 77

 13 omega   34.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -180.0000 64
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0296373000
_diffrn_orient_matrix_UB_12      -0.0543616000
_diffrn_orient_matrix_UB_13      0.0328080000
_diffrn_orient_matrix_UB_21      0.0017585000
_diffrn_orient_matrix_UB_22      -0.0711652000
_diffrn_orient_matrix_UB_23      -0.0773148000
_diffrn_orient_matrix_UB_31      0.0219794000
_diffrn_orient_matrix_UB_32      -0.0676449000
_diffrn_orient_matrix_UB_33      0.0550257000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17949
_diffrn_reflns_theta_full        72.48
_diffrn_reflns_theta_max         72.48
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.009
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89968
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5344
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         8599
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+13.2663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                7420
_reflns_number_total             8599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51301g.txt
_cod_data_source_block           meru
_cod_database_code               7023411
_chemical_oxdiff_formula         C9H10N2O3Cu1
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O50-H50 = O65-H65 = O3-H3A = O3-H3B
 0.84 with sigma of 0.01
 O35-H35A = O35-H35B
 0.84 with sigma of 0.02
 O28-H28A = O28-H28B
 0.84 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C34(H34), C38(H38), C41(H41), C43(H43)
3.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C54(H54A,H54B), C62(H62A,H62B)
3.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C36(H36), C37(H37), C39(H39), C46(H46), C48(H48), C53(H53),
 C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C63(H63),
  C64(H64)
3.d Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C1(H1A,H1B,H1C)
;