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_4340505
_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         'C42 H72 N2 Ni2 O13'
_chemical_formula_sum            'C42 H72 N2 Ni2 O13'
_chemical_formula_weight         930.44
_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             2013-02-10
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.088(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.2188(8)
_cell_length_b                   19.6774(9)
_cell_length_c                   10.4136(5)
_cell_measurement_reflns_used    4320
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      28.4413
_cell_measurement_theta_min      3.1646
_cell_volume                     4913.4(4)
_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      99.95(10)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -88.00  -43.00   1.0000    2.6500
omega____ theta____ kappa____ phi______ frames
    -      -21.3871  179.0000 -180.0000 45

  2 omega  -65.00   49.00   1.0000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       22.7933  -49.0000   60.0000 114

  3 omega  -69.00    6.00   1.0000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       22.7933  -77.0000    0.0000 75
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0039392000
_diffrn_orient_matrix_UB_12      -0.0151753000
_diffrn_orient_matrix_UB_13      0.0597811000
_diffrn_orient_matrix_UB_21      0.0249430000
_diffrn_orient_matrix_UB_22      0.0154132000
_diffrn_orient_matrix_UB_23      0.0304045000
_diffrn_orient_matrix_UB_31      -0.0154123000
_diffrn_orient_matrix_UB_32      0.0288415000
_diffrn_orient_matrix_UB_33      0.0152802000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9491
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.17
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86588
_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    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.279
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.086
_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     282
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0527P)^2^+14.2358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                4074
_reflns_number_total             5031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501036h_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4340504--4340507.cif.'
_cod_database_code               4340505
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H20 of C20, H16 of C16, H19 of C19, H18 of C18
 At 1.5 times of:
  {H5A,H5B,H5C} of C5, {H8A,H8B,H8C} of C8, {H10A,H10B,H10C} of C10, {H9A,H9B,
  H9C} of C9, {H15A,H15B,H15C} of C15, {H21A,H21B,H21C} of C21, {H13A,H13B,
  H13C} of C13, H7 of O7, {H3A,H3B,H3C} of C3, {H14A,H14B,H14C} of C14, {H4A,
  H4B,H4C} of C4
2.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C16(H16), C19(H19), C18(H18)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C),
  C10(H10A,H10B,H10C), C8(H8A,H8B,H8C)
2.c Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;