Mixed donor-functionalised phosphinomethanide complexes of the alkali metals; synthesis, structures, and solution dynamics
Wills, Corinne; Izod, Keith; Young, Jonathan; Clegg, William; Harrington, Ross W.; Dalton Transactions  (2009) 6159–; doi:10.1039/b903119g

data_7001754
_publ_section_title
;
 Mixed donor-functionalised phosphinomethanide complexes of the alkali
 metals; synthesis, structures, and solution dynamics
;
_journal_issue                   31
_journal_name_full               'Dalton Transactions'
_journal_page_first              6159
_journal_paper_doi               10.1039/b903119g
_journal_year                    2009
_chemical_formula_moiety         'C28 H49 N Na O2 P Si2'
_chemical_formula_sum            'C28 H49 N Na O2 P Si2'
_chemical_formula_weight         541.82
_chemical_name_systematic
;
?
;
_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                 99.349(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7246(16)
_cell_length_b                   21.945(5)
_cell_length_c                   12.9043(10)
_cell_measurement_reflns_used    95525
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      4.0
_cell_volume                     3276.1(9)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1148
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            77315
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         4.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+3.3118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                3354
_reflns_number_total             4251
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b903119g.txt
_cod_data_source_block           ki166_compound12
_cod_original_cell_volume        3276.2(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7001754