On the possibility of magneto-structural correlations: detailed studies of dinickel carboxylate complexes.
Walsh, James P. S.; Sproules, Stephen; Chilton, Nicholas F.; Barra, Anne-Laure; Timco, Grigore A.; Collison, David; McInnes, Eric J. L.; Winpenny, Richard E. P.; Inorganic chemistry 53 (2014) 8464–8472; doi:10.1021/ic501036h

data_4340504
_publ_section_title
;
 On the possibility of magneto-structural correlations: detailed studies
 of dinickel carboxylate complexes.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8464
_journal_page_last               8472
_journal_paper_doi               10.1021/ic501036h
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '1(C40 H58 N4 Ni2 O9)'
_chemical_formula_sum            'C40 H58 N4 Ni2 O9'
_chemical_formula_weight         856.32
_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             2013-02-10
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.358(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.7520(4)
_cell_length_b                   20.1962(5)
_cell_length_c                   42.5463(10)
_cell_measurement_reflns_used    16984
_cell_measurement_temperature    105.5(10)
_cell_measurement_theta_max      28.2630
_cell_measurement_theta_min      3.0960
_cell_volume                     9231.1(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      105.5(10)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.8735
_diffrn_measurement_details
;
  1 omega  -51.00   63.00   0.7500   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0746   77.0000   60.0000 152

  2 omega    0.00  117.00   0.7500   80.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000  150.0000 156
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0635163000
_diffrn_orient_matrix_UB_12      -0.0078313000
_diffrn_orient_matrix_UB_13      0.0033364000
_diffrn_orient_matrix_UB_21      0.0133412000
_diffrn_orient_matrix_UB_22      0.0341083000
_diffrn_orient_matrix_UB_23      0.0024069000
_diffrn_orient_matrix_UB_31      -0.0123007000
_diffrn_orient_matrix_UB_32      -0.0034422000
_diffrn_orient_matrix_UB_33      0.0161651000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            36116
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         18841
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+19.8189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                13977
_reflns_number_total             18841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501036h_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4340504--4340507.cif.'
_cod_database_code               4340504
_chemical_oxdiff_formula         C42H72Ni2N2O13
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H31 of C31, H29 of C29, H30 of C30, H32 of C32, H33 of C33, H24 of C24, H25
  of C25, H26 of C26, H27 of C27, H28 of C28, H43 of C43, H42 of C42, H41 of
  C41, H40 of C40, H39 of C39, H80 of C80, H76 of C76, H84 of C84, H83 of C83,
  H82 of C82, H74 of C74, H75 of C75, H77 of C77, H79 of C79, H78 of C78, H38
  of C38, H34 of C34, H35 of C35, H36 of C36, H37 of C37, H86 of C86, H87 of
  C87, H88 of C88, H89 of C89, H90 of C90, H85 of C85, H81 of C81, H71 of C71,
  H72 of C72, H73 of C73
 At 1.5 times of:
  {H23A,H23B,H23C} of C23, {H22A,H22B,H22C} of C22, {H21A,H21B,H21C} of C21,
  {H19A,H19B,H19C} of C19, {H20A,H20B,H20C} of C20, {H18A,H18B,H18C} of C18,
  {H70A,H70B,H70C} of C70, {H69A,H69B,H69C} of C69, {H4A,H4B,H4C} of C4, {H3A,
  H3B,H3C} of C3, {H5A,H5B,H5C} of C5, {H9A,H9B,H9C} of C9, {H10C,H10D,H10E} of
  C10, {H8A,H8B,H8C} of C8, {H68A,H68B,H68C} of C68, {H66A,H66B,H66C} of C66,
  {H67A,H67B,H67C} of C67, {H65A,H65B,H65C} of C65, {H46A,H46B,H46C} of C46,
  {H51A,H51B,H51C} of C51, {H48A,H48B,H48C} of C48, {H47A,H47B,H47C} of C47,
  {H52A,H52B,H52C} of C52, {H50A,H50B,H50C} of C50, {H14A,H14B,H14C} of C14,
  {H15A,H15B,H15C} of C15, {H13A,H13B,H13C} of C13, {H62A,H62B,H62C} of C62,
  {H61A,H61B,H61C} of C61, {H60A,H60B,H60C} of C60, {H57A,H57B,H57C} of C57,
  {H55A,H55B,H55C} of C55, {H56A,H56B,H56C} of C56
2. Restrained distances
 C20-C17 = C17-C18
 1.44 with sigma of 0.02
 C20-C17 = C17-C18
 1.55 with sigma of 0.02
 C20-C17 = C17-C19
 1.55 with sigma of 0.02
 C19-C17 = C17-C18
 1.55 with sigma of 0.02
 C66-C64 = C64-C67
 1.55 with sigma of 0.02
 C67-C64 = C64-C65
 1.55 with sigma of 0.02
 C65-C64 = C64-C66
 1.55 with sigma of 0.02
 C20-C18
 2.352 with sigma of 0.04
 C20-C18
 2.532 with sigma of 0.04
 C20-C19
 2.532 with sigma of 0.04
 C19-C18
 2.532 with sigma of 0.04
 C66-C67
 2.532 with sigma of 0.04
 C67-C65
 2.532 with sigma of 0.04
 C65-C66
 2.532 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
H1A ~ H1B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
H10B ~ H10A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C22) = Uanis(C23) = Uanis(C21)
Uanis(C69) = Uanis(C67) = Uanis(C70) = Uanis(C65) = Uanis(C68) = Uanis(C66)
Uanis(C49) = Uanis(C45)
Uiso(H10B) = Uiso(H10A)
Uiso(H1A) = Uiso(H1B)
4. Others
 Sof(C45)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=1-Sof(C23)=1-Sof(C23)=1-
 Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-
 Sof(C23)=1-Sof(C23)=1-Sof(C23)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C69)=
 Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=1-
 Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-
 Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=Sof(C46)=Sof(H46A)=
 Sof(H46B)=Sof(H46C)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)=1-Sof(C23)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 1-Sof(H48A)=1-Sof(H48A)=1-Sof(H48A)=1-Sof(H48A)=1-Sof(H48A)=1-Sof(H48A)=1-
 Sof(H48A)=1-Sof(H48A)
5.a Aromatic/amide H refined with riding coordinates:
 C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C85(H85), C81(H81),
 C71(H71), C72(H72), C73(H73), C80(H80), C76(H76), C84(H84), C83(H83), C82(H82),
  C74(H74), C75(H75), C77(H77), C79(H79), C78(H78), C38(H38), C34(H34),
 C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
  C28(H28), C27(H27), C26(H26), C25(H25), C24(H24), C33(H33), C32(H32),
 C31(H31), C29(H29), C30(H30)
5.b Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C61(H61A,H61B,H61C), C60(H60A,H60B,H60C), C57(H57A,H57B,
 H57C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C10(H10C,H10D,H10E), C9(H9A,
 H9B,H9C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C23(H23A,H23B,
 H23C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C18(H18A,H18B,H18C), C70(H70A,H70B,H70C), C69(H69A,H69B,H69C),
 C68(H68A,H68B,H68C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C65(H65A,H65B,
 H65C), C46(H46A,H46B,H46C), C51(H51A,H51B,H51C), C48(H48A,H48B,H48C), C47(H47A,
 H47B,H47C), C52(H52A,H52B,H52C), C50(H50A,H50B,H50C)
;