First Row Transition Metal Complexes of 1-Methylcyclobutenedione, a Monosubstituted Squarate Ligand
Bert D. Alleyne; Hazel-Ann Hosein; Hema Jaggernauth; Lincoln A. Hall; Andrew J. P. White; David J. Williams; Inorganic Chemistry 38 (1999) 2416–2421; doi:10.1021/ic981011k

data_4321999
_publ_section_title
;
 First Row Transition Metal Complexes of 1-Methylcyclobutenedione, a
 Monosubstituted Squarate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2416
_journal_page_last               2421
_journal_paper_doi               10.1021/ic981011k
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C5 H15 N Ni O12'
_chemical_formula_weight         339.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 114.929(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.5473(7)
_cell_length_b                   14.671(2)
_cell_length_c                   7.2687(11)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.91
_cell_measurement_theta_min      6.17
_cell_volume                     633.15(15)
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2061
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        4.16
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.594
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0245(27)
_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   1.064
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1916
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.075
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_obs          0.0262
_refine_ls_shift/esd_max         0.966
_refine_ls_shift/esd_mean        0.049
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.2287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0749
_refine_ls_wR_factor_obs         0.0726
_reflns_number_observed          1767
_reflns_number_total             1916
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981011k_2.cif
_cod_data_source_block           LH9702
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.2287P] 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^)+(0.0392P)^2^+0.2287P] 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        'C5 H15 N O12 Ni'
_cod_database_code               4321999