Temperature induced single-crystal-to-single-crystal transformations and structure directed effects on magnetic properties.
Legrand, Yves-Marie; van der Lee, Arie; Masquelez, Nathalie; Rabu, Pierre; Barboiu, Mihail; Inorganic chemistry 46 (2007) 9083–9089; doi:10.1021/ic700867b

data_4333388
_publ_section_title
;
 Temperature induced single-crystal-to-single-crystal transformations and
 structure directed effects on magnetic properties.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9083
_journal_page_last               9089
_journal_paper_doi               10.1021/ic700867b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C10 H16 N2 Ni1 O10 S2'
_chemical_formula_sum            'C10 H16 N2 Ni O10 S2'
_chemical_formula_weight         447.09
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-06-14
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_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.50596(10)
_cell_length_b                   12.56344(15)
_cell_length_c                   8.66640(11)
_cell_measurement_reflns_used    7592
_cell_measurement_temperature    95
_cell_measurement_theta_max      33
_cell_measurement_theta_min      4
_cell_volume                     809.342(18)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      95
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.027
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_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11334
_diffrn_reflns_theta_full        30.171
_diffrn_reflns_theta_max         32.794
_diffrn_reflns_theta_min         3.738
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  30
_diffrn_standards_number         '4 frames'
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_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
AbsPack - CrysAlis RED (Oxford Diffraction, 2002)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       prismatic
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_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0931
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.001117
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 50.8 -75.3 54.6 -20.8 6.89 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0263
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_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2316
_reflns_number_total             2788
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          6.982(9)
_oxford_structure_analysis_title mih11
_cod_data_source_file            ic700867bsup4.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Adding full bibliography for 4333385--4333393.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C10 H16 N2 Ni1 O10 S2'
_cod_database_code               4333388