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_4322000
_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            'C10 H14 Mn O10'
_chemical_formula_weight         349.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.230(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8258(8)
_cell_length_b                   16.1527(14)
_cell_length_c                   9.9084(8)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.01
_cell_measurement_theta_min      5.25
_cell_volume                     1410.3(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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4344
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        6.38
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.5757
_exptl_absorpt_correction_T_min  0.4905
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       Prisms
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0238(14)
_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   1.048
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4109
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_obs          0.0376
_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^)+(0.0473P)^2^+0.3065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1058
_refine_ls_wR_factor_obs         0.0973
_reflns_number_observed          3303
_reflns_number_total             4109
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981011k_3.cif
_cod_data_source_block           LH9602
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.3065P] 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^)+(0.0473P)^2^+0.3065P] 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        'C10 H14 O10 Mn'
_cod_database_code               4322000