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_7012459
_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            'C30 H65 As Li N3 P4'
_chemical_formula_weight         673.59
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 96.165(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2635(3)
_cell_length_b                   15.4835(5)
_cell_length_c                   24.3220(4)
_cell_measurement_reflns_used    25511
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     3842.78(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_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      180(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28746
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  0.8061
_exptl_absorpt_correction_T_min  0.7905
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         8768
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+0.5309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                5935
_reflns_number_total             8768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211037g.txt
_cod_data_source_block           dw0032
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012459