Reactions of metallated cyclohexyl phosphine (CyPHM) with As(NMe2)3; synthesis of [(CyP)4As]‒ anions (M = Li or Na, Cy = cyclohexyl)
Bashall, Alan; García, Felipe; Hopkins, Alexander A.; Wood, Jody A.; McPartlin, Mary; Woods, Anthony D.; Wright, Dominic S.; Dalton Transactions  (2003) 1143–; doi:10.1039/b211037g

data_7012458
_publ_section_title
;
 Reactions of metallated cyclohexyl phosphine (CyPHM) with As(NMe2)3;
 synthesis of [(CyP)4As]-- anions (M = Li or Na, Cy = cyclohexyl)
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1143
_journal_paper_doi               10.1039/b211037g
_journal_year                    2003
_chemical_formula_sum            'C34 H68 As Li N2 O P4'
_chemical_formula_weight         726.64
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.204(4)
_cell_length_b                   19.464(6)
_cell_length_c                   21.771(4)
_cell_measurement_temperature    293(2)
_cell_volume                     8138(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       theta/2theta
_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  0.1123
_diffrn_reflns_av_sigmaI/netI    0.2982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            5296
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   psi-scans
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4317
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      0.851
_refine_ls_R_factor_all          0.2643
_refine_ls_R_factor_gt           0.0822
_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^)+(0.0326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1438
_reflns_number_gt                1457
_reflns_number_total             4317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211037g.txt
_cod_data_source_block           sx468
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7012458