Bis(phospha-adamantyl)alkanes: a new class of very bulky diphosphines
Gee, Victoria; Guy Orpen, A.; Phetmung, Hirihattaya; Pringle, Paul G.; Pugh, Robert I.; Chemical Communications  (1999) 901–; doi:10.1039/a902434d

data_7110551
_publ_section_title
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 Bis(phospha-adamantyl)alkanes: a new class of very bulky diphosphines
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              901
_journal_paper_doi               10.1039/a902434d
_journal_year                    1999
_chemical_formula_structural
PdCl2(C6H4O3Me2(CF3)2)P(CH2)3P(C6H4O3Me2(CF3)2).CHCl3
_chemical_formula_sum            'C24 H27 Cl5 F12 O6 P2 Pd'
_chemical_formula_weight         985.05
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 102.419(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.142(2)
_cell_length_b                   11.987(2)
_cell_length_c                   22.167(3)
_cell_measurement_reflns_used    7771
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.88
_cell_volume                     3410.3(9)
_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  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART area detector'
_diffrn_measurement_method       'narrow frame \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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17177
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(14)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.885
_refine_ls_goodness_of_fit_obs   0.906
_refine_ls_hydrogen_treatment    'see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7769
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.013
_refine_ls_restrained_S_obs      0.906
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_obs          0.0251
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0656
_refine_ls_wR_factor_obs         0.0558
_reflns_number_observed          7078
_reflns_number_total             7771
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902434dsup1.cif
_cod_data_source_block           3a
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0000P] 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^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3410.4(9)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7110551