Unique Group 1 cations stabilised by homoleptic neutral phosphine coordination
Marina Carravetta; Maria Concistre; William Levason; Gillian Reid; Wenjian Zhang; Chem.Commun. 51 (2015) 9555–; doi:10.1039/C5cc03184B

data_7117231
_publ_section_title
;
 Unique Group 1 cations stabilised by homoleptic neutral phosphine
 coordination
;
_journal_name_full               Chem.Commun.
_journal_page_first              9555
_journal_paper_doi               10.1039/C5cc03184B
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'Na P6 C30 H48, C32 H12 B1 F24'
_chemical_formula_sum            'C62 H60 B F24 Na P6'
_chemical_formula_weight         1480.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_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
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                79.047(4)
_cell_angle_beta                 78.403(4)
_cell_angle_gamma                81.625(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5084(10)
_cell_length_b                   16.4798(10)
_cell_length_c                   17.5637(10)
_cell_measurement_reflns_used    10011
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     3460.2(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from \w-scans'
_diffrn_radiation_collimation    'Confocal mirrors, HF VariMax '
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31294
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.35
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ SuperBright'
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.7651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         13561
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+2.1072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                11050
_reflns_number_total             13561
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5cc03184b2.cif
_cod_data_source_block           14r911a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7117231