A simple route to multifunctional phosphide and amide donor sets; syntheses and structures of [{ButPAs(NMe2)2}K.pmdeta]2 and [{CyNAs(NMe2)2K}2]∞
Beswick, Michael A.; Hopkins, Alexander D.; Kidd, Sara J.; Lawson, Yvonne G.; Raithby, Paul R.; Wright, Dominic S.; Bashall, Alan; McPartlin, Mary; Rothenberger, Alexander; Stalke, FT3Dietmar; Chemical Communications  (1999) 739–; doi:10.1039/a901222b

data_7110492
_publ_section_title
;
 A simple route to multifunctional phosphide and amide donor sets;
 syntheses and structures of [{ButPAs(NMe2)2}K.pmdeta]2 and
 [{CyNAs(NMe2)2K}2]\\infty
;
_journal_issue                   8
_journal_name_full               'Chemical Communications'
_journal_page_first              739
_journal_paper_doi               10.1039/a901222b
_journal_year                    1999
_chemical_formula_sum            'C34 H88 As2 K2 N10 P2'
_chemical_formula_weight         927.12
_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                 105.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.014(3)
_cell_length_b                   12.750(3)
_cell_length_c                   15.014(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     2585.4(10)
_computing_cell_refinement       'Stoe control software, DIF4'
_computing_data_collection       'Stoe control software, DIF4'
_computing_data_reduction        'Stoe software, REDU4'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe four circle'
_diffrn_measurement_method       'omega/theta 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  0.0985
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3473
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         4.09
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.5765
_exptl_absorpt_correction_type   'Psi scans'
_exptl_crystal_colour            'Dark orange'
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1468
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                1956
_reflns_number_total             3357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            901222bsup1.cif
_cod_data_source_block           dw9817
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7110492