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_4310581
_publ_section_title
;
 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            'C22 H26 Ni O14'
_chemical_formula_weight         573.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.580(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6536(5)
_cell_length_b                   8.3936(9)
_cell_length_c                   22.297(2)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.67
_cell_measurement_theta_min      10.58
_cell_volume                     1244.8(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_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      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            2135
_diffrn_reflns_theta_max         64.94
_diffrn_reflns_theta_min         3.97
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.769
_exptl_absorpt_correction_T_max  0.9966
_exptl_absorpt_correction_T_min  0.9056
_exptl_absorpt_correction_type   'Lamina (0 -1 1)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       needles
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0004(2)
_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_all   1.108
_refine_ls_goodness_of_fit_obs   1.190
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         1740
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.187
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.5693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1253
_refine_ls_wR_factor_obs         0.1104
_reflns_number_observed          1384
_reflns_number_total             1963
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic035193gsi20031015_051854_7.cif
_cod_data_source_block           Compound8
_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.

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^)+(0.0557P)^2^+0.5693P] 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^)+(0.0557P)^2^+0.5693P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C22 H26 O14 Ni'
_cod_database_code               4310581