Synthesis, Structure, and Magnetochemical Analysis of Selected First-Row Transition-Metal Anilino- and Anisolesquarate Compounds
Patrice M. T. Piggot; Lincoln A. Hall; Andrew J. P. White; David J. Williams; Laurence K. Thompson; Inorganic Chemistry 43 (2004) 1167–1174; doi:10.1021/ic035193g

data_4310577
_publ_section_title
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 Synthesis, Structure, and Magnetochemical Analysis of Selected First-Row
 Transition-Metal Anilino- and Anisolesquarate Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1167
_journal_page_last               1174
_journal_paper_doi               10.1021/ic035193g
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C20 H24 N2 Ni O12'
_chemical_formula_weight         543.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4167(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.4987(3)
_cell_length_b                   9.2437(2)
_cell_length_c                   40.2057(14)
_cell_measurement_temperature    150(2)
_cell_volume                     4606.3(2)
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            9232
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.9307
_exptl_absorpt_correction_T_min  0.7718
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Pale blue/green dichroic'
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       'diamond plates'
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3687
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_obs          0.0340
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+4.1243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0850
_refine_ls_wR_factor_obs         0.0775
_reflns_number_observed          3157
_reflns_number_total             3864
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic035193gsi20031015_051854_3.cif
_cod_data_source_block           Compound_3
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+4.1243P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+4.1243P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4310577