Synthesis and coordination chemistry of ortho-perfluoroalkyl-derivatised triarylphosphines
Croxtall, Ben; Fawcett, John; Hope, Eric G.; Stuart, Alison M.; Journal of the Chemical Society, Dalton Transactions  (2002) 491–; doi:10.1039/b107390g

data_7702706
_publ_section_title
;
 Synthesis and coordination chemistry of ortho-perfluoroalkyl-derivatised
 triarylphosphines
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              491
_journal_paper_doi               10.1039/b107390g
_journal_year                    2002
_chemical_formula_moiety         'C48 H28 Cl2 F26 P2 Pt'
_chemical_formula_sum            'C48 H28 Cl2 F26 P2 Pt'
_chemical_formula_weight         1426.63
_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-97
_cell_angle_alpha                78.74(1)
_cell_angle_beta                 77.80(1)
_cell_angle_gamma                88.85(1)
_cell_formula_units_Z            4
_cell_length_a                   12.280(2)
_cell_length_b                   18.509(2)
_cell_length_c                   23.735(4)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.37
_cell_volume                     5170.1(14)
_computing_cell_refinement       'XSCANS (Fait, 1991)'
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        'XSCANS (Fait, 1991)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker p4'
_diffrn_measurement_method       'omega scan'
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20707
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.008
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
based on 104 psi scan data (XEMP; SHELXL-97) R~int~ 0.0453 before correction 
and 0.0223 after correction.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         20219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.2371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                13740
_reflns_number_total             20219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107390g.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5170.1(13)
_cod_original_sg_symbol_H-M      P(-)1
_cod_database_code               7702706