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_4340506
_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_absolute_configuration ad
_chemical_formula_moiety         'C44 H66 N4 Ni2 O9, C2 H3 N'
_chemical_formula_sum            'C46 H69 N5 Ni2 O9'
_chemical_formula_weight         953.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.2042(10)
_cell_length_b                   10.7563(6)
_cell_length_c                   23.1759(14)
_cell_measurement_reflns_used    3305
_cell_measurement_temperature    151(20)
_cell_measurement_theta_max      28.4708
_cell_measurement_theta_min      2.8966
_cell_volume                     5036.6(5)
_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
;
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      151(20)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   34.00   59.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9183  179.0000  -30.0000 25

  2 omega  -46.00   60.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4027  -81.0000  -46.0000 106

  3 omega  -11.00   15.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4027  -57.0000 -120.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0161221000
_diffrn_orient_matrix_UB_12      0.0102347000
_diffrn_orient_matrix_UB_13      -0.0542871000
_diffrn_orient_matrix_UB_21      0.0083166000
_diffrn_orient_matrix_UB_22      -0.0287440000
_diffrn_orient_matrix_UB_23      -0.0164360000
_diffrn_orient_matrix_UB_31      -0.0300569000
_diffrn_orient_matrix_UB_32      -0.0024471000
_diffrn_orient_matrix_UB_33      -0.0336165000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.1172
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12471
_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    0.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90643
_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            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.030(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         6920
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+3.9495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                5113
_reflns_number_total             6920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501036h_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4340504--4340507.cif.'
_cod_database_code               4340506
_chemical_oxdiff_formula         C42H72Ni2N2O13
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H46 of C46, H47 of C47, H41 of C41, H43 of C43, H24 of C24, H32 of C32, H34
  of C34, H35 of C35, H36 of C36, H14 of C14, H17 of C17, H18 of C18, H20 of
  C20, H22 of C22, H23 of C23, H8 of C8
 At 1.5 times of:
  {H12A,H12B,H12C} of C12, {H49A,H49B,H49C} of C49, {H37A,H37B,H37C} of C37,
  {H38A,H38B,H38C} of C38, {H39A,H39B,H39C} of C39, {H42A,H42B,H42C} of C42,
  {H44A,H44B,H44C} of C44, {H45A,H45B,H45C} of C45, {H27A,H27B,H27C} of C27,
  {H28A,H28B,H28C} of C28, {H29A,H29B,H29C} of C29, {H13A,H13B,H13C} of C13,
  {H16A,H16B,H16C} of C16, {H19A,H19B,H19C} of C19, {H2A,H2B,H2C} of C2, {H3A,
  H3B,H3C} of C3, {H4A,H4B,H4C} of C4, {H5A,H5B,H5C} of C5, {H6A,H6B,H6C} of C6,
   {H11A,H11B,H11C} of C11
2. Uiso/Uaniso restraints and constraints
H1A ~ H1B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C19) = Uanis(C6) = Uanis(C5) = Uanis(C3) = Uanis(C4) = Uanis(C2)
Uiso(H1B) = Uiso(H1A)
3. Others
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-
 Sof(H2A)=1-Sof(H2A)=1-Sof(H2A)=1-Sof(H2A)=1-Sof(H2A)=1-Sof(H2A)=1-Sof(H2A)=1-
 Sof(H2A)=1-Sof(H2A)=1-Sof(H2A)=1-Sof(H2A)=1-Sof(H2A)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C17(H17), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24),
 C32(H32), C34(H34), C35(H35), C36(H36), C41(H41), C43(H43), C46(H46), C47(H47)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C49(H49A,H49B,H49C)
;