First-Row Transition-Metal Complexes of the 1-Methoxycyclobutenedionate(1-) Ion
Hazel-Ann Hosein; Hema Jaggernauth; Bert D. Alleyne; Lincoln A. Hall; Andrew J. P. White; David J. Williams; Inorganic Chemistry 38 (1999) 3716–3720; doi:10.1021/ic990199k

data_4322183
_publ_section_title
;
 First-Row Transition-Metal Complexes of the
 1-Methoxycyclobutenedionate(1-) Ion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3716
_journal_page_last               3720
_journal_paper_doi               10.1021/ic990199k
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C10 H14 Mn O12'
_chemical_formula_weight         381.15
_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                 97.094(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5651(5)
_cell_length_b                   13.2138(4)
_cell_length_c                   8.8586(5)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      11.21
_cell_volume                     1459.56(11)
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1274
_diffrn_reflns_theta_max         63.71
_diffrn_reflns_theta_min         4.88
_diffrn_standards_decay_%        7.98
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.990
_exptl_absorpt_correction_T_max  0.5846
_exptl_absorpt_correction_T_min  0.4281
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       Needles
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0009(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   1.057
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1216
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_obs          0.0411
_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^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1039
_refine_ls_wR_factor_obs         0.0960
_reflns_number_observed          1005
_reflns_number_total             1216
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990199k_1.cif
_cod_data_source_block           LH9706
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.0000P] 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^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_formula_sum        'C10 H14 O12 Mn'
_cod_database_code               4322183