Monomeric alkali metal complexes of a sterically demanding, donor-functionalised secondary phosphide ligand
Clegg, William; Doherty, Simon; Izod, Keith; Kagerer, Hartmut; O’Shaughnessy, Paul; Sheffield, Joanne M.; Journal of the Chemical Society, Dalton Transactions  (1999) 1825–; doi:10.1039/a900869a

data_7027306
_publ_section_title
;
 Monomeric alkali metal complexes of a sterically demanding,
 donor-functionalised secondary phosphide ligand
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1825
_journal_paper_doi               10.1039/a900869a
_journal_year                    1999
_chemical_formula_sum            'C22 H47 N3 Na P Si2'
_chemical_formula_weight         463.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                67.669(4)
_cell_angle_beta                 87.913(4)
_cell_angle_gamma                71.329(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5849(15)
_cell_length_b                   11.8767(18)
_cell_length_c                   14.424(2)
_cell_measurement_reflns_used    6725
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.25
_cell_volume                     1432.1(4)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.866
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10581
_diffrn_reflns_theta_full        28.81
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                4790
_reflns_number_total             6468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            900869asup1.cif
_cod_data_source_block           compound_3
_cod_database_code               7027306