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_4322185
_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            'C4 H4.5 Cu O6.25'
_chemical_formula_weight         216.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   16.2535(11)
_cell_length_b                   16.2535(11)
_cell_length_c                   8.1426(7)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.16
_cell_volume                     2151.1(3)
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2044
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        8.03
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.030
_exptl_absorpt_correction_T_max  0.6738
_exptl_absorpt_correction_T_min  0.5711
_exptl_absorpt_correction_type   'Face-indexed numerical'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_description       cubes
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0010(3)
_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   1.121
_refine_ls_goodness_of_fit_obs   1.167
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         1902
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_obs          0.0451
_refine_ls_shift/esd_max         0.015
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+3.5204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1219
_refine_ls_wR_factor_obs         0.1126
_reflns_number_observed          1537
_reflns_number_total             1902
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990199k_3.cif
_cod_data_source_block           LH9708
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+3.5204P] 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^)+(0.0544P)^2^+3.5204P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C4 H4.50 O6.25 Cu'
_cod_database_code               4322185