C2-Symmetric P,N Ligands Derived from Carborane-Based Diphosphetanes: Synthesis and Coordination Chemistry.
Coburger, Peter; Schulz, Jan; Klose, Jennifer; Schwarze, Benedikt; Sárosi, Menyhárt B; Hey-Hawkins, Evamarie; Inorganic chemistry 56 (2017) 292–304; doi:10.1021/acs.inorgchem.6b02173

data_4345157
_publ_section_title
;
 C2-Symmetric P,N Ligands Derived from Carborane-Based Diphosphetanes:
 Synthesis and Coordination Chemistry.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              292
_journal_page_last               304
_journal_paper_doi               10.1021/acs.inorgchem.6b02173
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C21 H36 Ag B10 F3 N2 O3 P2 S3, 1/3(C4 H8 O)'
_chemical_formula_sum        'C22.33333 H38.66667 Ag B10 F3 N2 O3.33333 P2 S3'
_chemical_formula_weight         819.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                83.519(2)
_cell_angle_beta                 89.019(3)
_cell_angle_gamma                89.103(3)
_cell_formula_units_Z            6
_cell_length_a                   14.7767(6)
_cell_length_b                   14.8998(4)
_cell_length_c                   23.7871(6)
_cell_measurement_reflns_used    8771
_cell_measurement_temperature    130
_cell_measurement_theta_max      29.3440
_cell_measurement_theta_min      4.7780
_cell_volume                     5202.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-2014/7
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130
_diffrn_detector_area_resol_mean 16.3560
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.1692
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
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_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            32868
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.529
_diffrn_reflns_theta_min         2.190
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93860
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; 
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       prism
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.784
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         32868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.784
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16448
_reflns_number_total             32868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02173_si_002.cif
_cod_data_source_block           12
_cod_depositor_comments
;

2020-05-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C67 H116 Ag3 B30 F9 N6 O10 P6 S9'
_cod_original_formula_weight         2458.93
_cod_original_formula_moiety         '3(C21 H36 Ag B10 F3 N2 O3 P2 S3), C4 H8 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        5202.4(3)
_cod_database_code               4345157
_shelx_shelxl_version_number     2014/7