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_7702357
_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            'C82 H106 Cu4 F24 N26 O10 P4'
_chemical_formula_weight         2449.97
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_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                90.0
_cell_angle_beta                 91.441(10)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   19.567(2)
_cell_length_b                   26.313(3)
_cell_length_c                   20.033(3)
_cell_measurement_temperature    173(2)
_cell_volume                     10311(2)
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.1153
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            63226
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_type   '? Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       needle
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.214
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1445
_refine_ls_number_reflns         23223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.214
_refine_ls_R_factor_all          0.1739
_refine_ls_R_factor_obs          0.0792
_refine_ls_shift/esd_max         -2.414
_refine_ls_shift/esd_mean        0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+21.6564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2000
_refine_ls_wR_factor_obs         0.1606
_reflns_number_observed          11581
_reflns_number_total             23223
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807599i.txt
_cod_data_source_block           /tintin3/people/elia/zoa/zoa
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+21.6564P] 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^)+(0.0641P)^2^+21.6564P] 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        10310.8(25)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7702357