Tetranuclear grid-like copper(II) complexes with pyrazolate bridges: syntheses, structures, magnetic and EPR spectroscopic properties
Mann, Karen L. V.; Psillakis, Elefteria; Jeffery, John C.; Rees, Leigh H.; Harden, Nicholas M.; McCleverty, Jon A.; Ward, Michael D.; Gatteschi, Dante; Totti, Federico; Mabbs,, Frank E.; McInnes, Eric J. L.; Riedi, Peter C.; Smith, Graham M.; Journal of the Chemical Society, Dalton Transactions  (1999) 339–; doi:10.1039/a807599i

data_7702355
_publ_section_title
;
 Tetranuclear grid-like copper(II) complexes with pyrazolate bridges:
 syntheses, structures, magnetic and EPR spectroscopic properties
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              339
_journal_paper_doi               10.1039/a807599i
_journal_year                    1999
_chemical_formula_sum            'C60 H64 Cu4 F12 N22 O4 P2'
_chemical_formula_weight         1701.43
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                85.254(10)
_cell_angle_beta                 70.087(12)
_cell_angle_gamma                68.15(2)
_cell_formula_units_Z            1
_cell_length_a                   10.410(2)
_cell_length_b                   13.282(3)
_cell_length_c                   14.170(2)
_cell_measurement_temperature    173(2)
_cell_volume                     1707.6(6)
_computing_cell_refinement       'SAINT (Siemens 1995b)'
_computing_data_collection       'SMART (Siemens 1995b)'
_computing_data_reduction        'SAINT (Siemens 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens 1995a)'
_computing_publication_material  'SHELXTL (Siemens 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens 1995a)'
_computing_structure_solution    'SHELXTL (Siemens 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       '\w rotation with narrow frames (0.3 degrees)'
_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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8183
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.934
_refine_ls_goodness_of_fit_obs   0.910
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         5820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_restrained_S_obs      0.910
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_obs          0.0360
_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^)+(0.0686P)^2^+3.0096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1056
_refine_ls_wR_factor_obs         0.0989
_reflns_number_observed          5409
_reflns_number_total             5820
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807599i.txt
_cod_data_source_block           /tintin3/people/ward/claire/kcu/kcu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+3.0096P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+3.0096P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1707.5(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702355