Structural and complexation properties of diselenacrown ethers. Synthesis and crystal structure of a novel cationic palladium tetraselena complex
Bornet, C.; Amardeil, R.; Meunier, P.; Daran, J. C.; Journal of the Chemical Society, Dalton Transactions  (1999) 1039–; doi:10.1039/a900545e

data_7027272
_publ_contact_author             'Jean-Claude Daran'
_publ_section_title
;
 Structural and complexation properties of diselenacrown ethers. Synthesis
 and crystal structure of a novel cationic palladium tetraselena complex
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1039
_journal_paper_doi               10.1039/a900545e
_journal_year                    1999
_chemical_compound_source
;
 synthetis as described
;
_chemical_formula_moiety         ' C16 H20 Pd0.50 Se2 O3.50 P1 F6 '
_chemical_formula_sum            'C16 H20 F6 O3.5 P Pd0.5 Se2'
_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_date             98-06-29
_audit_creation_method           CRYSTALS_ver_07-07-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.472(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8454(10)
_cell_length_b                   15.9185(15)
_cell_length_c                   19.7817(13)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      23.9
_cell_measurement_theta_min      1.7
_cell_volume                     4340.0(6)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_device_type  'Stoe IPDS '
_diffrn_measurement_method       \f
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13219
_diffrn_reflns_theta_max         23.96
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count 'every image'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    3.907
_exptl_absorpt_correction_T_max  0.5716
_exptl_absorpt_correction_T_min  0.5074
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       box
_exptl_crystal_F_000             2426
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.73
_refine_diff_density_min         -1.77
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.0725
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2589
_refine_ls_R_factor_obs          0.0414
_refine_ls_shift/su_max          0.027
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
; Robust-resistant weighting scheme (Prince E, 1982): 
 w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients 
 Ar(2.64, -0.407, 2.17) for the Chebyshev polynomial ArTr(x) where 
 x was Fc/Fc(max).
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0489
_reflns_number_observed          2589
_reflns_number_total             3316
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            900545esup1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

data name '_diffrn_measurement_device-type' was replaced with
'_diffrn_measurement_device_type' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        ' C16 H20 Pd0.50 Se2 O3.50 P1 F6 '
_cod_database_code               7027272