Complete and ‘incomplete’ [2 ×2] grids by self-assembly with a sterically hindered ditopic imidazole hydrazone ligand—structural and magnetic studies
Dawe, Louise N.; Thompson, Laurence K.; Dalton Transactions  (2008) 3610–3618; doi:10.1039/b800529j

data_7003847
_publ_section_title
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 Complete and &#x2018;incomplete&#x2019; [2 \\times 2] grids by
 self-assembly with a sterically hindered ditopic imidazole hydrazone
 ligand---structural and magnetic studies
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_journal_issue                   27
_journal_name_full               'Dalton Transactions'
_journal_page_first              3610
_journal_page_last               3618
_journal_paper_doi               10.1039/b800529j
_journal_year                    2008
_chemical_formula_sum            'C44 H52 Mn3 N28 O19'
_chemical_formula_weight         1441.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.283(5)
_cell_angle_beta                 80.327(5)
_cell_angle_gamma                86.514(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7348(13)
_cell_length_b                   13.6851(18)
_cell_length_c                   23.480(3)
_cell_measurement_reflns_used    10390
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      30.9427
_cell_measurement_theta_min      1.9810
_cell_volume                     3393.4(7)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34286
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.9334
_exptl_absorpt_correction_T_min  0.8627
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1478
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 222.3 electrons per
unit cell in one void (total volume 1001.4 A^3); that is 111.15 electrons
per formula unit. Four disordered nitrates appeared to be present prior to the
application of Squeeze, though a good point atom model could not be achieved
for these. The application of Squeeze gave a good improvement in the data
statistics and allowed for a full anisotropic refinement of the framework
structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0055(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         15289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0738
_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^)+(0.1519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2393
_reflns_number_gt                11165
_reflns_number_total             15289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b800529j.txt
_cod_data_source_block           shelxl_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Numerical' changed to 'numerical'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               7003847