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_4321998
_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 Co N O12'
_chemical_formula_weight         340.11
_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                 114.73(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.409(5)
_cell_length_b                   14.717(10)
_cell_length_c                   7.259(6)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.60
_cell_measurement_theta_min      11.68
_cell_volume                     621.9(8)
_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  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1493
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        5.34
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.7321
_exptl_absorpt_correction_T_min  0.2872
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       prisms
_exptl_crystal_F_000             350
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       0.0051(42)
_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   1.161
_refine_ls_goodness_of_fit_obs   1.197
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1277
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.986
_refine_ls_restrained_S_obs      1.193
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_obs          0.0638
_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^)+(0.0518P)^2^+6.2038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2971
_refine_ls_wR_factor_obs         0.1643
_reflns_number_observed          1142
_reflns_number_total             1373
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981011k_1.cif
_cod_data_source_block           LHCAN2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+6.2038P] 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^)+(0.0518P)^2^+6.2038P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        621.8(8)
_cod_original_formula_sum        'C5 H15 N O12 Co'
_cod_database_code               4321998